,

the ~sychedelic
<5uide to
l3reparation
ofthe
~ucharist
in a few of its many gu ises

as edited hy
/{oben E. Brown & Assoclatt:~
of the :-.Ieo Amcrican Ch urch Leaguc for Spiritllal De"clopmcnt
&
Thc Ultimate Allthority of thc Clcar I.ight
Ded icateo to A ldous Hu:dev and ali the coura-
gcous ind ividuals who ha~e CO Ille aftcr, lha t
dare to brave perscclItion in arde r lO bring a
li ttlc Light into thl: warld.

COP)" &n! 1%8

h)' Robe rl E Urlm "
Ali ri?ht ~ , t ~!\' cd
2nd cdition. 191 1
3,,1 e<l1! ion , 19 73
4th cd ltion . 197 5

Aùdil ionoll copi~s :l~ihble by Moot:y Or dcr trom :

Lin~..a Sha rirJ I nc-~n!t C".
P.O. Bl'X 43ì·1 . Austin. TCX ll :' ì~ 76 S U.S .A.
Priee (sllJpp lng indu dcd )' SUO
 11\TRODUCTION

T hi, bookkt con tai ns sl:l'eral procc ~ses con- Ccrtain of the proccsses a re gi\'~n in qui t .
cnni ng t lte Illan u facturc and. to soml' extcn t. tcchnical Il'rms \Vi t h li t t le ex pl:J nOI tinn or
Ihl' li se of \"arious halluci nogcnic chemicals. mi nu te òClail s. while othcrs ano ,illlrkr ami
Th l' -l' dwmic;JIs are ali rt!q ricl,!d by f"deral req uirc Illu.: h k ,~ know lcelgc of organic ' hel1l-
la\\' anò po ssc~~ i on or ~al' or most is defi nilely ical techn iqut: to sllccessflllly ca rry out thl'ir
ilkgal. d ir<!c li o ns. Th.: rc is a re~son for t!lis typr of
Prc~en la lion or 1hcse pro.:e,ses is (I.:s igncd I,! yout. SOIllI.! o f the Iècll niC] ul!s arc c, trcll1ç-
for pèrsons who know ho\\' to lise ha ll ucino- Iy compkx ami oflcn are tl:rri bly c13ngl'rOll';
gens ami wh o wi sh to use them fo r rc ligioll ' to an yon<! nOI ros,,:ssing :J. thorollgh kn owl-
purposes such as thc myslica l Psychedc li c edge of org~nic techniquc. 19noran l blunòt'r,
Expc ri c n c~ . Thc only o lh cr source o r tlll:SC could cause ccr tai n o f the produ\:I S to tllm
drllg. for n:ligioLlsly oric nlCd p.:rso ns is no \'! poisonou .. anel other proccdun:, use Chl'Illi-
the black markcl. ""hl' re mix tllr.:S of \':lriabIc cals so dangaou s tha ! fl a Ill ing cx p l o~io ll'
co,t 3nd ljllcst ion3 ole qU 31ity m:Jkè Ihè ha z- \Vo ultl bt! th' n:,ult of small Illi -ta:l.!s. Th,'
artl s of ll~ i Jl g tll<' ~l' aln.'Jtly tricky u rugs :l lmost yic lels in 1l13n y cases art' drastically rcdu.:·ò
prohibitive. if propc r kchn iqu,' :lIld .:quipm,'n t :Ire Ilot
Th csc IHol'c dur~; arI;! accuralC allli rcli:l b k uscel . Sincc ali of tll<,<;t' p roc.:s'cs art: lO ';0 111<"
an el product! purè prodllcls or ,uitabk quality extcnt chemkal proccdurcs. it is highly 3e1-
for :Illllost any usage rcquiring hi gh s tandarcl, vi sa o1c th:lt Jlly I:><!l;:on a t tcmpt il1g lO follo\\
of C]u<Jl ity. Thc c.:ompounds Ihus proeluced them \Vit h any hopt: cf ,ucc.:css sho dd bl' pro-
are k" likcl y lO ca use si(1<- e ffccls due lO fi,' knt in organic tCl' hnique and t heory .
impu ri tic, si ncc the quality 'a n be lll<Jck IO For thC~l' r.:ason s the Iri ck y ,md d:lIlgerous
appruacll I h:lt of pharmaceu lical housc pro- proccdmcs are .:ouched in terms òcsigned to
duc ts. d isc.: ouragt: thc un traiJh:u person .
 'l'ABLE OF CONTENTS

11'\T KODUCT IO ....... ..... ........... .

1\OT ES 01" EfI'ECTS OF I1ALLUCI :-IOC;E l S 01'1 THE MI:'\O .... . .... ......... ... . 3

PSYCHEDEI.lC DOSAGE IN FOlnIAT IO:-.i ........... .... . 5

ADJUST I 'G \VI TH OTHER ORUGS ... ................ .... .... ......... ............ ........ ......... ............... ...... 7

M!\RljUA 'A Cali Ila bis saTira R

Cu lt iv:lt ion of .\hriju ana ............ .... .. ... ..... . 9
Hashish ano Bhang ... ........ ..... .... ...... ................ . lO
Mariju ana Rcd Oil Extractioll .. .... ... .. ... ..... ... . l l
Synrhesis of THC-I.ikc Compounds ...... ...... ... .. 12

PEYOTE Lophoplror(J wi//ialllsi 16

Peyotc ClctuS Extr:H: l ion ...... ..... ... .. ............ . .... .... ......... . ....... ....... . 17
.\ \cscaline Synthcsis No. 1 .. ...... .. ...... .. .. ..... .. . . .... ................ . ............. . 22
,\ \cscalinc Synthes i, No . 2 .... ........... .. .. .... . .... ............... .... . . ....... . 25
.\Icscalin c Synrh csi, No. l ano ì\o . 2 Combincd . ............ .... .. ... .... .... . 26
.\1USIIROO.\ IS Psil()cybe SI'. 2S
Psilocvbin Cu lture 29
Svnrh'csi~ of Psilocvn .. ............ ... ...... .. .. ........ .. ............ ... . . .
32
S~ b stitu tcd Trypt;mincs .. .::::::.... ..::::::::::: :: ::.::::::." :.:........ . : ::: .:....... ... :: .: ..... :.. :... ........... . 36

.\ IOR1\I:-I(; CLORIES ('V/ll'o l1 'ullIs l'iol(/ceilt' .. ....... ......... .. 40

Ergot Culture and Ex tractio n 41
LSD . Thrcc Synrheses 43

STP 47
PH OCURE.\1 E1\T 01' NECESSARY IT EMS 48
II0MEI3UILT Lr\ B EQU IP.\1ENT 49
 NOTES ON TH E EFFECTS OF HALLUCI NOGENS
FRmf A PSYCHE DELIC VIEWPOINT

Th~ brain i$ an imlll~lb.:ly complex. r;ll1- lO m:J intain b~: d~\·elop in g . ;lt r andorn, a flow
domly co nnc: clc:d comp u l.::r. babnced ami of sy n ihd ic sc:nsory dala. Till.: mimi sccs th c:se
tlln ed by <In inlric;\ tc: c hcmi al ,\Ild c!cc lrica l synthcscs 3~ hallueinat io ll S, allei Sl'ns's lhe loss
,yslèm whirh heps il fllnctional l'v('n wh e n of the refc:n:n-=c eoordinalt:s in a fee ling of
scvcrl'ly damp..:d by alcohol o r s tim\lla tcd by llisoril'n tat ion with a lack of any concep t ion
:llllphdamin..:,. Howc:ver. rhe: highcr brain. the of rime. d ircc rion. d ime nsiono t.:!t:.
ecrcbral corl<:x. is tkpcmknt llpon a constan t This ranùorniz ed sta t ~ o f lh.: b r,li n may
Ilo\\" of ~nsory inpUI lO givc il a reìc rcllcc illas I nearly b~ likencd to tha t of a ncw-born
frame UpOIl whi eh it builds irs variolls opera- chi Id wll o Ilas no st abilily . due lo lhe :JIN:nce
lion$. Any di smption of Ihis Il o\\' deslroy, of any cooTd inales al ali oth.;r than inhc:ri(('d
the n.:fe r ' nce frall1 , :lnd Ihl' cerebrllll1 lcm- ins t incts. T hr muin diffcr<:nee is tha t a psy-
po rarily lose, ilS ab il ity to correla te dala . ehc c1c lically trea tcd bruin ha' wllat is ,'a llcd a
Any mdhod wh idl will mollify or s top the minù built up in its networks, whik u l:h ild
fccd of data lo the ce rebrum prodllCcs almos t is ernpty.
rhe SJmè d'fecI. Th e psycho logist's sensory Wc Ilavc sccn how rhe mind conti nues to
dcprivJ lion box. a physical syslcm, n.:lJ)OV~S iry to funclion ~\"en when thc fOllndal ions
ali SOliTe ... s of sc nsory sl illlubtioll . Cntai n have bcen c1 issolved. The foundalion , or frarne-
chcm ic a ls, t he ha ll \lcinogcns. mercly disrup t work , is known as the ego, the d iS$ol li tion 01'
the intlllx of sensory informa tion by \Inbal- which is conseq ll t'ntly known as ego-lo S. l f
,Illcing lhe low.::r brain where the st'ledion thc minc1 has careflllly bccn coached to accept
ce ntcr l'or ill co millg da t a is localed . giving a ego-Ioss, it will conti nu e to progrcss until it
jll mbkd ma,,-, of llnrccognizably e rossed sig· finally fr.:c s itsl:l f in its comp ktc fonn. The
n<lls. Uoth lllcthods kavc the highc r ecntcr rt'sult of lh is fin al inward look is a sclf-awarc-
with a 11 0;lling n:fcrcncc sys«' m whic h il tries ness and cnligh tenmen t which is dcvastating

3
 in im p ac l .mò unbe lievablc to a n yo ll ~ who h as anel wh icl! may apI car wil h ali th.:: Icrrifying
ne\' e r lInde rgonc Ihe sallll.: I!x perie nc', reality of thc origi nai cxpaicncc, ;\11 thal m a)'
T b c pe riod of ~go-Io:s and Ihen Ih' P ' riod ha\'c hpt Ihc m in d frolll psychosis 1ll3y ha\' e
or rd ll rn o r Ihe ego are very scnsilive lo been th ' suppression or those u nb;;arabk ex-
inIlucnc<=s t'rom Ihe ~n\' i ron m cnl. ci t hcr lO Ih e paiene!:" Unless th e Illood su rround ing the
good or lo Ihe d e trimen ! of Ih!;! indil'idua l's ~ts ion , is nc arh' idea i coupled lI'ith com-
m ind , The main ca u se o r Ihi s e,x In:-me sensi- pk lc tru s l in t lle Guru, th..: person ..:oul d
lil'ity lo o u tsid' slim ul i is Ilw sIate of no- brSl' in lo a lb:p p:;yc ll olic fuglll.: t'rom whicI!
fr::\Jll <=wor k as exis ts in Ihe infanl. Thi~ arti- I!' mighl n..: \' ' r rec o\'l! r. Vay skillfu l Il a ndlin)!
ficial r ' birlh or thc m ind ~holl i d be Irca lcd or a se,;sion 1ll3y vcr)' pO~'lbly bring lllo~c 'x-
wi t h :1$ tnll c h can:- JS Iha l gil'l'n lh l! in !'::lIl1 pè'ri.: nl'I.'s Ollt in ,l tr'IIl'lu il "t'tling wher ' t hl.'
m ind, wit h gre,llcsI care dcvotcd lo pn:li m in- Guru I11Jy Il elp l he "c rson ncutra lize Ihe
ary sc I :m d sdling for cach psychcdelic ex- Iraulllatic "ff.:c t pnlll3 n\:nlly,
p 'rienc.::. lt m usI :l lwa)'s be remcIllbercd h ol'l Ali thl.'se cO lbid.:-rations ,hollid be ':l rl'l\il ly
the dcepe 'I a nd 1l10- 1 significanl tr3l11l1alic loo k,' cl a flcr by individ1l31s seài ng r.:ligiolls
expcricnccs COille when Ib' m ind is la rgdy t:llligI Ht:llnll~n t Ihrough drll g,;, Lighl doses temi
unfoITlled. as in Ih,; carlil."1 ye : HS of life. lo <:nhan cl' Illood~ blll do n oI ll';u;!l!y init ia l":
O l he r cl angcrs in thl: dccp psychcdcl ic l'X- slron~ hallucinogenic re'lctions, a nel ;I r ' no t
p,'ricllcc d I'a li' l'rom dcc I' contlic ts and IraUm a:; as dangl.'fOtls, I lea\ y doses t1sed IO bring :lbOli l
whic h are kept hidùcn t'ro l11 lhc mind normally the psych e<k lil' ('xp'rie ncL' sho lld n,' v..: r be
ca.-1I :1Il y play..:d wilh by Ihl' no~ ice .

4
 l'SYCH EIJ ELl C IJOSAG[ IN FORMATION

Ali do~~gç infor mation which follo\\'s pur- traeks as sign, o f a hero in addic:t. :'>1ost im-
po~cly avoi ds I11cn tion or any mdhocb wh ic h portant. inj ectablc c1rugg Jl(:cd thc ca re and
inv o l\'1.! injl.!ctitl1l. cithcr intravt'llou; or intra- qual it y-con trol a\'a ilabk on ly in pharm:lcc u li-
mll ~clliar. Injec tion 'a n be un,afe ~~ far a' cal house sca le prodllc ti on. he nee are not
heal t h n:ason$ go and does Icad to easy deree- practical in th e ordi n3ry l:1b.
tion by la\'.' ofliee r$ who may in!t'rpret n 'T dk

DOSAGE HY WEIGIIT

Expcricnced Nu rmal Firsc "'taximum

Dru g Light Hi gh
U~cr Psychedc/ic safe dose

LSD 20-50 I-lg 100-200 I-lg 300 I-lg 400-800 I-lg 1000, 3000 I-l g
THC l mg 2.5 mg 5 mg 10 mg 20 mg
STP 5 mg lO mg 22 mg 35 mg 50 mg
m·n 5-10 mg 20-30 mg 'IO m co" 50-60 mg 100 mg
Psil ocyn 5-10 mg 20-30 mg 35 mg 40 -60 Illg 150 mg
,\kscd inc 50 -200 mg 300-500 mg 4 00 nlg 600-800 mg 1000 mg

Th c vç ry light doscs only gi \'e a fèe1ing 01' few cl n handi<.' plc;ls:Jntly. Th ~ sl ig ht toxie
well -bc ing allei sc::ldo l11 C:! lI S ' Illllc h hall ll -ina - sid.: df·cls ar(' nOI J 1ll3jor factor in co nside r-
lion . Th<' cxp<'rie ncl.!d u~cr ca n ac hk \'l: th e in!; th e d05<lgC becaust: th ' ha ll ucinogenic ' /'-
psydlede lk effce t \Vit h k$.~ or a dose . grading fccts an: so m ucl more ovcrwhe lming at those
01'1' to no drug at alI. :\ pl.!rson trying to l.! X pcri- high dOSè S Ihal otha faetors are minimizcd
ene(' the full psychedel ic cffl.!ct l'or t hl' f irst Thl' nude na tural substanccs are n ot li st 'd
time nccds lo bl' eliscon nected Illueh l1lor~ lI erl.! bec;llIsc th c al1l 0u llt of drug ava il:lblc doc~
fu ll )'. thl'J'~forc l he la rge r dose s, Tilc largcst nOl fo ll o \\' any rclia le wcight pi.'rec nl ~gc as
dosc\ c au se :1 eom pklç brt'a k wi th rt'ali ty th:ll l h<' q uality 01' th ese" 5ubsta nces is not al ali
constan !.

METHODS
;\11 rotl ~ l i\'~ ly saf<! m~ t hod s of dosagl! in- Ill UCOUS membrancs 01' thc dige s tive trael t3kc
\ o lve absorp tion th rough \omc of the IllUCO US in ali but D:'>1T dlìcknlly. THC and its eruder
Jllembranl.!s. LSD. STP , and m c caline sho u lel forllls. marijuana an d ha shish are fa I sol uble
nor b;; vapo riu d by heal 3S they de compost' and e nter mos l ,;l'l ìci~n ll y ii disso lvl.!d in
on heating. bUI the othcrs a rI.! more hea t slabk butter or cooking oil. wh ic h aets JS a c3rric r
and may be takcn in to the l ung~ as a vapo r. and cnters via t he ia t absorp lion proces . DMT
usually through SO Jlle form of sllloking. T hc anel THC cxcept;.:d. a li llle h alluc in ogCJl5 an:

5
 qUl' kly :I nu dtìc i ~n t l y absorbed into th. using fooùs or dr ink JS carrier" Care should
low(' r int~' _ ti n a l trm:l il' illl ro d ll L~ d by 11I'::II1S be taken to pro t ~.:t l.SD l'rom heat an d pro-
or a Yé :aline ~nçl1la, Esthl't ic:l ll y unplt'<ls:lnt lo nged expO'i url.' to :! l, I.'spcc:ia ll y in an aq ue-
:1$ this means of inlrodudiol1 rlI ay bI.' lO L ' l'- ous sol li tion, Ali ,rude produ ' l s ,hOll ld be
tail1 Jlcopl , il is 011 ' of thc mos t .-f'i,i(' nt 'ithl!r groun d l'cr)' fine or vaporized into
I1H::t hod" LS D i~ so po wcrt'1I 1 in tiny dos~~ :mokt:,
Ihat it Illay b' takcn Jn y Illllnb<:: r 01' \\'J ys

DOSE AD JU STMENT AN O BU I L DUP

Most h:lI luci nogc nic intoxiç;tlions may I ;: : mokcd) d':pl:lld larg~ly 011 t hc fu ll dose be ing
adjllsted hy t'urthl'r do.;ag" fol lowing tl!e ini t l31 absorbcd in O I1 C brcillh fo r J lo~ 1 c f fe ctiv~ re-
inf!cstion, It IllU,;t be remembered , hOI\ c\'L:r, ,ults, DM 'J' ~(lllll: t ime, fa lls cn lirely if tak~ n
thal th c ad l';lnlagl' or thl' initi al shoçk 01' t h,' 100 slowly,
drug will larg('ly b' 10' 1. cl iminis hi ng t h~' psy- O pti mll lll rep.:a t frequem;y of d rugs is dc-
dlt'dclic dfcct gr('at ly, Sim il;lrly, il' th,' do~agt! termincd by lhl! lt:'lIg.lh of tin1l' the body t:Jkc '
is rep eated 100 OI'len, th e body r 'mains SOI11,'- IO bccomc orI' I t ~ g lard lO Il!' full shock of
what on i t~ ,~lIJrd and aga in Ihc l''yche do:li' I h ~ llIin d-disoricn t ing dfcct. RccOI ay lime
;Illvan tagt: 1\ Icsscncd , lIallucinations \V ili bc apparcl1 tly is abau t 15 tl J11 CS the kn!!.l h of
pr "e nl. but should not be' 'onfIl Sl!d with thc thc intoxiçat ion 3nd is l:li tl ou t for sevcr:ll
flili. non-gamt!, F i r~ t l33rdo awakt.!ning, halludnogcns il1 the l abl ~ bdow, As body
D0'i3gc adju: lment i, f:lirly ~ i lllp i ' witl! ~ I ow d lt:mislril.'s vary the figufI,!s I~ !ll be :Jpprox i-
a 'tlllg , long tcrm hJlluci nogel1s , F ast· ~( t i llg l1I ~ tl:, 'o Olle 'hould nOI b~ wo concern cd il'
h3lluçinog.: ns Ich a DMT al\(I THC (l\' h':l1 recovcry tim '; or C\'CII uosag~ tolcranc('s vary
frOlli per 0 11 to p ' rso n,

JJJ'u g Length of Session Oprimllnl Rc pea t Fre(lucncy

D,\!T 15 mi nu tes c\'cry four holll's

T I-IC (s l11o kcd) 3 hours daily
TI-IC (e:lien) 6 hou r. tI 'ice lI'eek l}'
Psilocvn 6 hours rwice week ly
l.S D 12 ho urs week ly
IIlcso linc 12 hours wcckly
STP 24- 36 hours m'ice mol1t hly

6
 ADJUSTING WITH OTH ER DR UGS

Olh~ r drugs sho uld be used with grt!al ca u- tirncs hc ighten cd . Nial:ill:uni,k (3 g) ,md a, -
tion. Sea sicknes5 n~mcdi '5 lik e Dr;Jmamine will w rbic ac id (3 g) combined will abort a bad
Iwlp combat na usea. Librium c;llms ncrvous LSD tri p in abo lt an hOllr. :-'1 o noso diulll glutJ-
indiv id uals in the pre-sl'ss ion periodo I f Sl~ \' l.! rC Illa t ' has ;} slight effcl:t in rcpairing menl3 1
(ra lllll;! dl'"dops and none or the verba l IOne after a session.
m Clho d ~ work. t he n ch lorpromazinc or o thn B1BLlOG RAI'HY
ph 'noth iazinl' tran<] u ili zers m a)' be lIsed to Leor}' . I. ; ~Ic(zncr. R.; "nd :\I pen. :\ . The P"'chc-
stop thl' hallucina tory e ffec ls. Th is should Il o t drlic Exp cnc ncc.l'\cw YorkThc L'nil'ers ill' P rc~,. 1964.
"Chemica l 3nd Engll1cc ring .'II C\\ s" Vol.' 4 6. No. 12.
be Llse u wi th ST1' as (he effccts are some- pp . 32-38 .

7
 CU L1W ATION OF M A RIJ UA :"I A

,\\ ar ijl1 alla gro\\'s in almos! any c1i mal<:. bl1[ to show cli fft' rcnt ia tio n imo male! and km3k.
prcfcrs a hot period at thc end of thc gt'OWillg T li c, l'l'male plalll'; . whic h hal'c the most tctra-
se:mm . I t \: f O W S best in loose, fertile soil, bu t hydrocann abinol, :tre slU rdy , Jark grecn bushcs
wi ll survi\' ~ in :thl0St any h3sie soil. prc::fcrab lv Sl'I'L!ral l'.: C l lall with lea!y brac ts ali over thc
with aJequatc fertilit }' an ct Illoiswrc which :tre llppcr sl~l11, hidi ng thl' fl'lIIale Ilow-:rs and
casily pro\'i\lcd . Thc !ap roo! goes dce p, so the s"d~. l' h, i1Idlc plalll s b"ome ' oJl1cII'hat lall
soil shoul d have ~ dc:pth 01' :1( 1e:1St three fcet and ,pindl y ~ lId ar~ light .: r gr 'en , \Vith t h ~
:I1 l O\'t' iJcJrock.
l11ale grl' cJ1i,h-Yl'llow nowns d;JJ1 glin i! In the
S~b: ! ollly ll l<' b~SI s~~d. Wil d m~rijualla brl'c7.c, 1-131.: plants. to derive an)' good l'ro m
is uSI>:! lly 01' .1l1 inf~rior slrain, ';0 'l' kct scc ct thcl11, I11 m t bl' lak.: n a l first ,ign 01' thl'ir
l'ro m il good Indian slr;lÌn or fro/11 tlll' b~Sl f1owns. Wh.:n th ~ kl11; Ji ~ nowa, hav-: bloOI11-
.'\capuko Col d. SOl11l' ,c~(b l'rol11 l'lIred mari- cd anel b,t'ore' lhe' sceds have sc t, th;H portioll
jU;ln:l may b~ nOlll'iabk . ,0 caeh hal ch nlll,1 , lio ulLi be ha rvcslcd, remale nOwL' rs are ha rd
be t\.!sled by gcrl1linat io ll 01' ;1 s:J1I1p k in il IO SCl: ami 1I1l1,t be cxamincd close ly lO fo l-
rolJ.::c1, damp tO ll'cl se t in :1 warm plal'c l'o r il 1011' th ei r progr<.'ss.
kw day s. l'ick thc uppl' r Ieal'l';, bract s, and f10wers
WhL' 1l d;lI1ger or l'rosI is over, pianI lhc sel' ds [rom lhe feI11;Jil' pl;lnls. Dry in a warm w~ lI -
I.~ illClt liL'CP ;lI1d lhn:~ illc he, :Jparl in \l'cII 1·L!J1 tilal<.!d pl acc , prd'a:J bly no l in dire cl sun-
l11 11khl'd . wdl tllrl1ed. ,Iighlly basico I\: rli il: lig hl. Whcn th oroughly drictl, thc JI1 a teri al is
soil. T hc sl'cd, \Vi II b" \I P in about th rl'l' days , ck;lI1 cd aliti CUl t'o r ~ lII ok i J1 g. 'l'o kec p 3ny
at which til11e tlit.:y mu st be wat chcd so lha t Icngth 01' time. ,cal in an airtight container
slugs. isopods an cl cu tworms do no t l';lt [henl. Wil h 5':", by we ighl of 9 5 ~; l't hanol (E\'crc1car),
A rta Ilte >ccdlings ar~ lwo \\'l'd;s olcl , li ttk The Fede rai N:lrcot ics brigadc doesn'l Iikc
car' i, IlC '(kd to protec l lhcm , as the hcmp pcopJc lO grolV mar ijuan:l in the Uni tcd Sta les
pian t is ex tr<.'l11el y h;mly. Th i.' secds may be ;md will am;! ~ l anyOJ1t: wlto all o w; thc planl lO
<Iartl'c1 in indiv iduai contai ners IIIdoors ;JJ1d grow on his propcrry. Man )' tilllL's mcler
sc I 0111 wh cn lh <, y havc a good start. rt.: ~ (krs are ins twr tl'd to look fo r m a r iju ~n3
II' thc plalll~ bcgin to sho w exccssivc hcigh t, and rl'po rt \'ioi3tors to thc I3lJrc;1U. It is stili
thl' Y may be:: toppe d by pim:hing lhc ~pica l possible lo grow 1l1'lrijuan a in ~kx ico. allhough
bud, maki ng them grolV bushy rath er lh ~ n mos t "r~as h;l\'è ~por;jdic~ lI y enfo rectl laws
talI. bt" in thc season thc pl:ln ts will bcgin rc gardin g il.

9
 HAS HISH
A!\[) BHA:"J(;

Il hal1ì,'. i, the d ricd, nud" wate'r ç':-; Irac:{ ur I h~ "X Ir,lct m u('h ca~it: r, 'l'hl: ,0h'CI1 I is eV;'1'or-
t hL hl'mp pl 'lnl. Ca1l/labis saliv.1. Tili , producI at l: d ~n d lhe h :ls hi~h sh:lp"d inl o b locks, i\
is cOlll illonly preparcd in ,a,; \c m cOlln lri.::s >t:,'ond t::-;Ir: lcl sho ul d b' m ad,' 011 c:lI.: h ba k h,
t'ro m both low am i hi gh gl'ad,' p l :lllt~, l'k nli- Ih(' solwnl from Ih.1! go in g in lO l'r~ sh pbn t
fui r:l W m:ll<'ri:d is :\\',Iil:\bk in lilc innullh:r- III J ll: rial as th,' IIr, [ l:~ tr:ll'l SOllll ioll, i\ Ihird
:Ibk h, mp fll' ld s or IhL CCII tra i Unit<:d Slatc" , ,':-;lracl ma)' b.: m:ldt:, th:1\ so lv,'nt b~illg sa\' c' cI
IlIdi,1l1 p ro,','sso rs g:\t h" r Ihe \l'h o i<: pbnb :I , Ihc sù: ond ' xtf;lèl Solu li on l'or J lIll th<: r
al til li e or !lowcrillg, 'Ind with no fun h" r tre;][ ' b:lt (' h, TI1<' so:ll,ing [i me ,hOll ld b..: :11 1e:1,1
m,'n! tile planr m:trcri:J! is nl:lcer:lled in :l ov~rni g.hl l'or bes I res ul ls ,
cru,hn-ro lkr Slm ilar lo Iha! us,d in suga r For USC, Ihl' Bh ang or Iws h ish sholl ici be
CIIIC p rll,c"in).!, T ll<' (l'w,h,d hl'mp i" q,' ' Ih'd ph y,ica ll y lllodili.:cI sim:.: th,' , 01 id bio..:).; fo r m
iII boiling waln wilh a(kquat' sti rr in)! 'o a, lo is ,Irl in cft'icicn t fo nn cith cr to l'al or lO Slllok c,
I!::.ch Ih,' ,us J1 l'ndabk so li b t'rom th ,' fibrous The b lol' k h :{,hi~h nw y b ~ ,h:l\(:d \','it h a sh3rp
:l1ld \l'oody pOrlion<, ' I Ìle llI ur ky , g rn~l1i,h knit',' , o r. if :1 I:I rgc quanlily 0 1' Bha ng is in-
,olli li on i, ,illlmc r,' d , Iow ly lO rc' clu ,:c th c l'oll'ecl, the makri :iI may be CII I Ihill ",ith :l
volum,' , a nd Ih ,' ,yrupy r.: ,idll" is dr i ,~ d in Ih,' hOl knif(', :lried in ~ 100'C O\'en, :lIIJ p ll l\'er-
"un or in a drying 0\', 11, Th,' r,',u llill g lII as, b ized iII :1 hkndcr. l' o\\'dcrcd Hh :mg is c :lsily
ro lk d ililo 1IIIIIpS or Illokkd int o blocks for bkndc d inlo smokin!! m ix tUf,'S , or :111 a koho lie
,;i1 ,' , 1111, producI is ma li e lo bL dis,oh cd In a tilk't ur, of has hish or bhang m:l}' b~ l11:1d..: by
dri nk hUI it is ,old fùr h:" h ish in the Ulliled uking up thl' ,;olub k porl ions inl o fo ur lim.:s
S tatcs, lIa shi sh i, mad,' by ru bb in g th" sticky Ih e Wl'i ghl or \\'arm <)5',; (' thyl ak:o ll o l.
gr,'c' n p b nr" then Ili bbing th L h amb lo 1'011 l' o 'lCti\':llC h:1Shish o r b ha ng (o r l11:uiju ana)
IIp the ,Ii c ky rl's in, l'h i, is Illol dcd in IO blocks, and lO prcpare it t'or usc in cook ing, simply
..\ more pr:.dil':ll l'rocc,, iII thi, country h,'H the Can nabis prepar:llion with thc fat
,'o nsi,ls or drying th,' pianI> :md str ipPlIlf! Ilw dcsircd in ,111\' rccipc. pl liS a littk \V:ltc r,
!l':IVCS :l nd tlo wl'r, trom tl w la rg,> ste lll', T lti, Thl:n si ill lllcr lhc mixlurc cat'l'fu lly 0 \'<:1' lo\\'
k :!Ì'y Illal 'fi:d " l'a.:).; ' d inl o :1 Jargc jllg or h.:al l'or ":\'Lr:iI IIOlIrS , being ,'3 rcfu l no l lO
ba rre' l ala] soaked with ei lhl'l' ;: k ohol. an:tonc scordi th e tn:ltl'fi:lls, Th, oi ly port io n \ViII
or a puri fi cd pd rokll lll so l\'t' nl. I l' mally ,~eds ha\'l' turncd a n ol i\'c gl'l'l' n am1 \l'i li h:wc m ost
31',' prt'Scnl tlh' pt:lrOk ll1ll so lv ~ nl shollld no t of thc :lCti\'c prin ci plcs d issoll'ed in it, This
be IIsl.' d, A si pholl ìi!!'d with;1 slr:lint:r p u t in mt' thod tr ip!t:s the eHicieney of h ashish uscd
Ih ' cOll lJi n,'r b,'l'o r..: l'illi ng mak,'s r..:mo\':t1 0 1' for ca ting purposcs ,

lO
 J\IARIJUAr\:\ RED Ol L l:XTRACTION

'[ h~ t'CIlWil: flo wers ,! nd kafy top,; :I r~ c<.ll- lighter tl uids or il g:lsol inr typ.: _ hig hly \ 0 1.1-
I - ' t~d bdo r ~ t h, "Tlb have ,~t. Ik Sll r ~ to ti le ck:1I1ing fluid. l'he extract is lì ltcr..:d :IIHI
ury it in J p laL~ with aU~4 11 3t - \ -ntila tioll IO conc.:n!ratt'd by <!v:lporat io n or car,' flll di, -
pr,'\ <.'n t molding . No curing is nel'c"a ry in prc- !illa tio n_ taking great "::Ire l O :ll'o id an.' !lame
p~ri nf! m3r ij u3 n3, as thc st rc ngth of thc prcp- in the vicin ity_
aration i~ cntircly dcpc nd cll t on th c \',l rie ty The gUl11my (k posit ohtain.:ò I, q lll !':: po-
!,:rOll'il . In this pro(;:ss :my f!raòe. CVt'n wi lò kn!. bUI fUTtha puri fic;l lion b possibk. Stealll
mak ri,J!, m:!y be us.:d incc it is IO b~ COIKèn- d i~t ill ation rcmol'cs the adorali:; terp n lL's. l'hl'
tral ed ami a !Joor grad ... l1lC'rcl y gil' l's le" yil'ld driecl rl'sin Imy tllen be clislilkd al 5 x JO-3 1ll 1ll
]l(' r I)()Uncl. Hg prcssure. <:olh: ( ! the t'raetion BP 70 .. 100·
l'h,' dri.:d . grounò Imkria l is .:x tr:ll'kd re- anu stop 1\'1 1(: n Ihl.! re ~i d lll.! bl.!gins lo li '..:om-
pcatedly lIsing ,I hydro ~:l rb on soh'cn t prcf- pOSI.! . 'l'h " di ·Iill:ttl.! is Illarijuall:! reti oil , \'l!ry
crab!\', al though aJcoh o l i~ 'l>mr times used _ activl' ph ysiolog.ic3 11y_
.-\ 101'1 boili llg ,011''':lI t i~ most cOI1\'(' nienl sinn: B111UOr. R:\PlIY
it is r"'lllov~d t'rom th e ~xlra cl mast '::Isily_ JO\l rn.l l oi Ihc Amene.1n C'hemicJI S" c idyj~_. 1%.
The 1ll0st eco llo mica l sol n .! nl i, ont' of th,' Jotllnal 01 I h~ Amrrican Chcmic,,1 Socict ; 6 2. 2 1')<;.

11
 SYNTH ESlS OF TETR AH YD ROCANNABI OL TYPE COMPOUNDS

Th~ synthesis of tctrdhydrocannabi nol is SY:'IITHES lS OF S-ALKYL RES ORC l l\' O LS

\ls\lally sOlllewh3t tricky il' intermed iates are
not a\"ailablc. Thl! esst:ntial portions of th' Any of the 5-a lkyl resorcinols ma)' be sub-
molecule which must be obtaincd for the stituted for o livetol in the se methods. In Ihe
fina l condensa tion are an isoprcne scries cs- rollowing proccdures. along with olivetol, is a
senti~1 oil. sudl as pulcgone or citral, and a5- compkx synt hcsis 01' a 5-alkyl re sorci nol which
alk yl n:sorcinol. The latter compound is Ie,l I will giw an end produ 't which is 50 timcs as
eOllllTlOIl ami most likdy to bl: watched . <leti\'c as the na tural producI.

PROCEDU RE l - One of thc most direct OLi VETOL

synlheses is a one step procedure, slirring 18g Stcp I -- 3, 5- Oinitro But)'1 Phenone
o li vetol with 15 g dIraI in 100 m i benzene at
5-10 tkgrel.!s. containing IO mI 01' boron tri- Prcpare the grignard r~age nt from 50 g 1-
ìluorid,' dhc ra le. The rcal!tioll should pru- chIaro bu tam: by retluxing with 20 g m3g-
cccd une hour, then tbc rnixlurc is cXl ra cled nesiu m turnings in 500 mI dry e ther sol ution.
wilh dilulC alka li (l ';t sodi ulll hydroxide) lO Take prcl'autions cOl1l;crning ct ht!r fumc:s l'S-
n::mo\"e ll ll: un reacted o li l't:tol. T o puriry . caping anel air entcring thl' nask by fastening a
chrolllarograph on a ìluorisil colum n with long tube l'rom the ret1ux conde nsa to t lll;
hexanc IO rcmuve the first iSOIllCf whidl i ' o utsidc air . A cryslal o r iod ine may be ncccs-
inacti\'c. buI not poisonous. Subsequcnt "Iu- sary to in iti atc tht! rt'a c tion. Whcn the r 'ae-
lion with a 9:-5 solutioll of hexane-db ' r will tion is compi 't.:. add 92 g anhydrous caclm ium
bring oft' two m o n.: isom~rs loget her, one 01' chloridc anel co ntinu I! the rdlux anoth..:r 15
which is ae tive. The solvcnt solution. when to 20 mi nut es. 'l'he ~[her is remov' d using
evaporated, le3\'CS a rc sinous resid\le vcry vacullln :md to Ih..: rc-idual Cd compl..:x is
sim ib r. il' not idl:nti ca l. to the 'l l! tive compon- added 500 mI bl.!nzene. taking ca re to keep
cnts in mariju3na in very cum:cn trat ed form o cxccss oxygcn out since the compound may
spon tancously tak..: !ìrc in air. To this mix-
PROCEDURE Il - This me thod llses pukgone ture is ad ded 115 g (0.5 r.lo1t.:) of 3, 5-dinitro
instead or citral. and bu tyl lithium as t lw benzoyl l!hloridt:. Reìlu:\ for 15 minu tcs and
mcalls of effeeting tlll': co nden sat ion. distill ofr the be nzene. Reco\'er the ketone
To bUly! lithiulll prt!part'd from 2. 5 g using dis lillalio n under redllced pl't:~~un:: . tak-
lith ium and 20.5 g of anhydrous n-h u tyl ing thc: !argcst fraction.
ehlorid.:, add 42 g 01' dry methoxylated o li ve-
tol. carrying out thc rca-:tion under nitrogcll STE P Il - 1(3. 5- Dihydroxy) Phenyl Penta ne
gas. Afte r shaki ng fo r three hours. 25 g (26 .8 Prcpa rc the Clemmensoll zine by dropping
m1) or dry pulego nc in 50 mI 3nhydrous c ther mollen zinc in water. Immerse 160 g or thc ~c
is a dd~d and fifteclllllillules later Ihe mix ture granules in :l 5 ~~ mercuric chloridc solution
is cautiously decom posl'd with ice wa ler. Ex- for t wo hours. Decant and rinse wilb \V3t~r.
tract with et hl![. Dbtill at I mm after the ether Piace the 3ma!gam and 62 g <0.25 Mole) of
and \Vater art! takcll 01'1'. The mcthyl groups 3. 5-dinitro butyl phenonc in a large nask an d
may hl' rcmoved by warmi ng an alcoho lic add a mixturc of 400 mI \Vater and 200 mI con
soIution with hydriodic acido HC I. Atta e h a renllX condenser alld gently

12
 11ea t th e mixture u n l il a " igorou. rC:lcrion minlltl.'s. Care must bc taken lo kcep the te m-
s t ~ rts. \\' he n thc rcacrion has slo we·d. ( an- pe ra ture lo\\', 63 g (47 m i) mOTI: dimethyl
ti nUl? Ille r.:ll\lx fo r t hr\!c m o r~ hO\lrs, adding sull'a te nwy thcn be added, alIowing thc tem-
15 m i o r con IICI t'vay ho ur. Rc mo"c the perature to r ise ro 45 degrees, R efl ux this
unspcnt am a l ~am . cool alld a dd 50 111 1 con
sulfuric a, id anel 50 g 01' sod i\llll nitri te kt'c p-
mix tur~ fa r o ne hour. al which time I m i of
5()<,~, sodium hydrox ide m ade up to 25 mI is
°
in g th c ll:m pera t lIr,' Il car I :) de grt'es l'o r tb.: added and rc ll u x is co ntinued anothcr hour
fÌrst bai f bO\l r. !\ 1I0 w t hl' tc m pera t lIrC to ri st' lo saponify any ester Iha! may be iormcd ,
to 95 de!!r..,es a nJ he:!t ar rhat tl' m pe r ~lturc l'o r Coo l the so luti on a nd ac id ify with con HCI.
2 hOll r" E:>.t ract th,' o livet o l with t h rc.: ot: n- VaCllllJll li lrcr rhe i c ~- co ld so lution a nd dry
ze ne wa ,h l·s. [O': 1110\'e the bell / e lle a nd pllri l y tht: precipilal è in warJll a ir.
hy d is t ill al ion :t ll d ull d a n: d \lcc d pre ,slI rt' .
Q
BP 18 0 a l 6 mm . STEP III - 3, 5-0imethoxy Bcnzoy l Chloride

A IIIGIILY ACT I VE EXOTIC To 500 g of 3, 5 dim e thoxy benzoic acid o

add 31 () mi freshl y di t ilIèd (pure ) rhionyl
5-ALKYL RESORCINOL
chloriJe :Illd he31 t he mixture two hOllrs in a
S fE P I - 3. 5-J)ih ydroxy lknz o ic Aciel wat<?r oa th. Th l' m ix ture is dis tilled u ndcr
redll ccJ prcssurc using a li gla ' joinls. Yicld
T o a ~u , pc n s i on o r 130 ~ pmvt!e r,'d iro n ill is 510 g, ooili ng al 150 degrecs ( 18 mm),
500 m i I\at ' r ( o llt~l i ni n g 40 m i c on il ei is
:1(.J(ft-d 100 g 3, :; d ill irro l '1I/.0Il' :lc id a lld th l' STEP IV - 3. S-l) imcthoxypheny l 2 mcthyl
m ix t lire i ~ rc rI \lxl'd fa r tll'O hOUl'. Th,' :Kid i . hepr:mo ll c
\:ru Je an il illc lkril' atiw i: li lll'n:d a nd t he Ii i-
This stt p is a Grign;ud rèadi o n and lhe
rratl.' ar idi !ied wi th I () ) mi ,' Oll ,u lfur iç a, itl
a p pa rallls should h al'e a lo ng \'e nt lu be l'rom
an d 7 :' g \odi u m nit rik i, inlrod ll .:(' d . Thc
Ihe rcll ux 'o nJc nscr IO Vl'nt etha fUlll es alld
rc,l c t io ll ,ha ll Id be kc pl ne :! r ." - 10 Jq:rcl's fo r
p rel' cnt :Iir l'ro m cnkring the reaclJon , A
OIW h:"! hOIll" \\'hen Ihe' .;o lu l io n i, , Io wly
- oupl.: of io din ..: eryst a ls help lO inili a tc a
broll gh r ro 'I:' dc)!rcl's :lIl d 1ll'ld :11 that lc'm lw r-
balk y r~a (;\ i o n .
al m , l'o r OIlC hOllr to Iho roug hly d l'è oll1 po'e
134 g ( I Mole) o r dry 2 chiaro heptan~ is
Ihl' d ialon ill ill sal t. f' ,l r:tèl tll c pro d ull \l'i l h
rctlllxed with 24 g of Mg t\lrnings in 500 mi
se\'t'fal w:I'hi n!!, or l' rh 'r. Rl' Il HWl' t hl' .: tl w r
:lI1 hydrOlis dh\!r in ~ 1000 m i RH Ilask lI nti l
an d r ,' cry~[3 I1i z ' the 3, 5 di h \'dro, y b 'Il / oic
t he re3crion is complete . Co o l this so luti o n lo
ac id froJ11 hol J k ohol.
-65 d ' grccs wilh a d r y ice <ll:l:tol1e balh and
adJ ~ 5 g anh y drolls l'ari e c hlorid e. To thi s
STEP " - 3, 5- Oi mc r ho~y Bl'll/o ic Acid
'old m ixt un: add 107 g (0.5 Mo le ) of t he
2 ); or' ~()di U Ill sulti re ( o r :1 nil ro);en Il ush) 3,5 di m t;lho xy oC I1 LOy l dl lorid ' from re p
is add n .l IO a 10 0 m i RB fb sk co nt a ining III. Slir l'o r scveral hou rs a t -65 dégr~es a nd
500 m i c al ci 1'/:11,' r wilh 60 g U:i2 mi 50'·1{ ~() I ) a l thl: \:nd al' t his period ade! fin <! ly grollnd
0 1' sod illlll h y d rox iJl' and the Ila" k i, liglt tly icc, all o wing rhe temp era rure to r ise l O 25
s toppl' rl' d and sh;lke n f(lr IL'n minute '. T o d..:gr..: ' , . R"!1l oW th e e ther and r ~c ol' cr Ih c
th is 'o lu l io n is rap idly add ed ì7 11 (0 ,5 ~ I o k ) kdon .: using dis till <llion lI ndcr rcd uced prc s-
o r 3 . S di h yJrux y oellzoic :ll:id. Whell thi; sur<!. la k ing Ihc I ~ rgè ~ t fr acr ion. Any te rria ry
so l\l tion i, d i ~50I\' e d, (;00 1 Ih e fl:t ,k ill ;1 co ld aIcoh o l pro dllccd IIla}' 01:: lI sed as is o r may
wal er ba t h . (i 3 g (47 m i) o f d im c lh y\ sull'a te oe Tt' duced to Ih.., alk.:n.: by passing o\'e r p u re
is [!tC Il added an d t h,' fh sk , tirred far 20 ac tiva lcd al umi na a t 350450 d.:grcc s, wit h

13
 ,ub,cq ucnt rcdu c ti on wilh sod iu1l1 anù ah-
sol ute alcoho l. This clcri\'ati\'l:. whik not :JS
plltc nl ;H the main prod ucI. is a l kasl a
STEP V I - 1(3 . 5- Dimethoxyphenyll
:.td ivc :JS ol i\'~t o l.
I. 2 Dimethy l Heptanc

STEP V - I 1.l.S -Oimet hoxyphenyl\ l. 2 Dissoh,,' the ùry hepknc cI.:ri\·ili\'c in abso-
Dimeth)' l l Heptene Iute: L'thano l ;md rcduce to th e 5-al ky l meth-
oxylakù rcsor:inol witl sodilll11 md:ll. For
Dry Ihe ke lollc o\' er anhydrou$ ~ocl i ul1l
the tct rahydro c:I nn:.t bino l proc<'dur~ I. rcllux
,ul !'a t.: . Prcpar-: 3 methy l grigna rcl reage' nl by
the produ c t wit h hyùri odi c :!L' id lO n:m ove the
rcad ing l)5 g (54. 7 mi l)r O!ll: \1 ok) or J11 t; lhyl
meth oxy groups.
hromicl ' with 20 g Mg !lIming,; in SOOml ~n ..
hyelrou d hc:r:l l a low te mpe ra ture (m ~t hyl
bromid,' bo ils ;It 3.56 lkgrcc,» . 150 g 10.5
1\'l o h;) or Ihc kc ton c l'rom st 'P IV i, c011lbinc ù
with this mC't hyl gri~ n :\f(1 r <?:l~~ nt anel th e
B1BlIOG KAPIIY
olu tion is rdlllxc d l'or 15 minu tl's. whc rcupoll J ùurn " l o f lh,' "" \('ri,'J I1 Ch<mlcal Soci" ' )' 88. 367
I DO mi or \V:Iter cOrl laillin!( I 1111 or COli ' lI l.. Journ::d of thl' :\n,,'nC'.:ln Chcmical $oci t.:l Y 62, 2204 .
t'uri.: a, id is added . Thc 1(3. 5 dimC'thoxy· ~56t'
Sh irk y. n.,.,.id .-\. Qr&l ~j~ R ~J~tio:), R, Cha p. ::. p. J I
phe nyll I . l dllnd hy l h" pt<-!l . i, disti l!.?d after
!\"lk: . Or gJ~l i~ Chcllli>try. S,'.:o nd Edit i" n. p. 152
the l'l he r :lIld waler h:!,; :dl pa,)Sl'd 01' t'. BI' Fi o" ' r 3ncl 1-i ~ sc r. O.I5:ln ic_ çhellli< ' ry . Thi:d Ediiion
:1hO Il I I SO dl:!,.'l'l·C'. "I
l' . i

II
JHC
\
I/ O
O

+ 0
H
1
O

Ol ivetol
C,H"

(o r aBy ', · Alk yl

I1c.o rcinol )

14
 OliVGtol

Il
() O
\ li
C

JCE~,
+
Ethe r
I ~ .,

Il
C, Il, ,
I
CH . C Il

(" (J

S-A!!"}'I
f{csort..lno!

15
 -- -
~,--­

~--
Q. -o

- ----::::=--
 PEYOTE CACTUS EXTRACT ION

The mature planls are dug or cu t pr.:f.:rably To pr.:pan: the pian!. make lhe slice (scc
al the end of the dry st:aSOll befon: thc rai ns r igure I ) '/z inch l elo\l.' tlh: lin\! whi,h sl.!par-
bcgin. The plants apparent ly use tlH: nil ro- ates the gre('1l to p frolll the roo t bark . Tito..:
g..moll' :l lkaloids ill gro wth when adcquatc sliced ofr bud,; stili have th at \/z inch of upper
rain is availabk. Con,;eqll~nlly the ~nd of a rool (overed with usc less cell ul ose 3ml dirl,
long dry ,peli i: besl, ,0 much .- 0 tha t yidcls wh idl i' rt:mov<:d by pin.:hing off chunks 01'
clrop bdow 50~-;' if plJnts are han'l'sled in a the hard bark from thl.! lough. nacçid plant
\Wl limi: . Cac ti thrivc on k rt ik soils rich in body, ]{insl.! tlte pian I, bricfly to ro.:mo\'o.! loos '
nilr gt!n and planb frolll go od soils onse- d irt and slill a\'oid leaching thl' plant malaial.
quelll ly produco.: c~tra alka loilb. Old large Do nO I bOlher \'Iilh th é' co t ton )' tu fts: th..:y ar..:
pia n" also giVl' lhc b.:,t yicld. a nui,an(;~. but not enough lo warrant re-
'1hc plant is shaped li kc an icc-c re:lm eone; 1ll0\'31. If pIJnts aro.: kcpl an)' h:ngth 01' lime.
the eone l'art being the rOOI :lnd thc ice-cream trcilt th~!l1 by sprinlding wilh naph Ihaknl'
being the gr<.:<:n :tlkaloid-ladcn top of thc plant. nake. Remove thi s preserva ti\" th orOl ghly
Thc root cOl1tains mo~t l ~1 carbohyd ratcs and il' the planh are to be llSed fr(:sh. This basi"
cellulose so that thc ver)' qnall amount of tro.:'lllllcnt i, the ini l lal ;,kp lO ali ot her pr,'-
lIlcscalinc obtained tht:rdrom is :lllllost impos- para tion proçe,s..:,.
sible to cxrract. Sinec on :r 99% of the alka- If th.: ..:aeli are lO be ston,'d 3$ .:rude plan t
loicl, ;Irc eoorai ned in thc gn:cn top and sincc 1ll3tcri,t1, th;:y ll1Uo;( Il(' dri.:d. Ev,n lh..:n thl'Y
rhe cellulose bulk reduccs the extr;letion yicld, will r<!tain po t 'ne )' only up lO two y..:ars. Thc
thc rOOI ma)' be rcmon:d with lin le reduction best procedun: fo r drying the buds i' to t:rllsh
in, and probabl)', an inc rcasc in yie ld . Ii thc th..:m bl'lw('..-:n woocl ancl dry thelll in th e ~1I11
roor, are !cfr in thc grolllld, morc pl ants will or in an OVOI at 120-170° r . Sun drying works
grov,:. besl il' thl' di1ll3te i, d ry, but :1 kikho..:n ()Vl'n
turnecl do wn low with 111t' door open \VIII
work . The drinl buds !lIay b..-: ,torl'ò thi .; wa)'
or may b~ ground to f10UT . SOlllclIlll 'S Ihc
..:ottony tuflS ar' sifl'd aut al1d IhlO' powder
is en..:a psulato..:d. 1I0w('\·l'r. 1110' would ne..:d
bctwl.!en 18 and 25 :;.-000 o.: apsult:s full lO gl'l
400 mg cquivalenl 01' Illo..:scaline. An alI 'rna-
tivt: wou ld be IO Illake up 8 g of the powòl'r
into a ;olu lion :lI1d lak, il :1> :1Il l'n":!l1;1. 20 g
al' powda l'qual I g of mescalinc.
The cactu . is ofttn takc n in ils r3W state and
chokl'Ò down, bUI due to bad :3 nd bitta
navor, eou plcd wi th the cmc lic :l tion of thlO'
drug. othl:[ me thod, are sO ll gh t. The ,implesl
01' these in\'olvcs making :3 pulp of lhc grecn
pianI III a blcndcr and diluting with lime jcl-
lo. tOlll 310juicc or other Illaski ng agt:nts. I-h:re
FIGURE 1 :tg:lin Ih b ' -t solution is lo USi:: an ':lI~ma.

17
 i\ t b('~t thl:sl: dosi ng mcthods arI.' :In ordeal th rou gh dol h as in *2. Re- holling 15 minlllc ,
for 11l0sl pt:opk, and lll any met hod s 0 1' con- in :I 5111311 am ouni of ac iùitìL: cI walc:r Iwo or
cl' nlr3lioll olher lhan drying (from thc In- Ihrcc limcs r,' mo\'cs ali poss ibk alka loids l'o r
dian ; ') havc b 'cn e!cvclopcd , Thc laboratory ~l1l y o r Ih"",; Ihrce mt'lhods. nl<:r, i, 110 11 l'l:d
pro(; cd urc has always bcguil \Vit h (he dr ic e! lO cu I up IhL: pian I, in ~ i lh <, r ;;2 or * 3 SI11 CC
groul1 d plant s. Thcs.: plant; an.' extracled wilh lhl: IrL: ~l t11l ": 111 Iea\" s Ih ' pl:lIlt mate ria l li kl' a
\\' ~ rrll akohol containing a sn1311 portion 01' spo n)!l' . Do nOI O\L'Tl'()ok . J) j'l:ilrd lhe ' Jl<~n l
NH .. OH (O.S~i:) . 111C Iiq uid is rh cn st raille:d bu ds.
off. lhe: solve n t rl:l11ovcd by d istillatio n, :lI1d Tht'''t' pro c:nlurc, n<:l a bi llt' r liquid . TlllS i,
thl' res idue trca tce! (or sepa ration into co m- ort ' n clrunk 5lr3ig.hl. 111ixcd, !!.: lI ed or takl' n 3,
pOIH:n t alkaloids. f or u~e , thc talTy residue :111 ,'n..:ma . l' he: bu lky pu lp has bcc n rc mo\'cd
may be l'alleò in cornstareh imo a ropl: amle n- bu t Ihe liql1id VOIU111<: i, sl ili .1 pro hlc11l . CL:11 1k
.:aps.li atcd. or Sl' nt to thl' llex t SI:lgc 01' con - boilin!! or simm t' rin!! \l'iII red ucI.' Ihl' \ ' o IU11lL'
':CI1( ra Iion ( s l~e fol lowing d i,clIssion). ')0',; or mOIL:. A r e$i no u~ . -l1m may form o
The che:a pesl and qllic ke~ 1 mdhod 01' Irca l- Skim. \Va,h lh' se um by lll ixi ng ",il h ho l
illg till.: c~l:! us i, \Vale r ('xtraclioll of Ih.:: fr.:, h wate r. slrain and S3ve Ih ... wJ ,hings. U,illg a
or Jn,d planl makri:lI by :111)' nll mbcr or fan :Ind an I.! I ' c:lri . sli rn:r will spc:cd evapora-
l,·chn iqucs. T hè main obj l:(;li\'t: is lo disrupl li o n whik kf.'e:p ing Ih .: I l'mp c>ralll r,~ lo w<'f. Thl'
Ihc cl: 11 wa ll,. ,'(llllbilizl! Ihc al ·aloid s. a nd COIKI:111ra le:<! li q llid \ViII kl!L: p il ft!w da y" wilb
remavI: lh,'m in ;) wa It: r ,ohi tilln from Ih" I ':é h,'n /l'm' ,hak,' n in a, a preso:r\'a li vL'. Th i,
'e:lIl1 losl' residue' :b qu ickly :J1ld l'fficicll ll y a, is uscd a n i}' in t'urllI 'r 'X lr:! ·lion. llowL:vl: r.
pos,i hk . Ali spills are so p ~lt'd IIp and n:tur1ll'J S0111,' wi,h III I 'ciUCI: Il (() lar 311 d lIS,' i or
l'or l'OIl IIIl11Cd lr"a 111lL!11 l il1 Ih" cur n;n l slL:p. SlOr' il lI1 Ih<.' t'orm or' a t.ir. In this ,:l,O: do
T hl' alk:lloi ds ar.: susccplihk {Q hre:a kdown by noI add a pl t's,· r\'a livt'. bu I t~\'apor3tL' it lO 1M
mo lùs, h3l:lL!r i:1. hea t, an d a.:i d or ba s, hydro- imllle:d i:lll'ly . Six or SL'vL:n ;;:00 c:!psu l ' S ,on-
IY'15. I herd'orl' thc fo llo win g lL' dl1l iq l1~s: lain a11ll ()SI ,.\00 mg of mesca lin,'. A cO:l 1i ng
(~\' k.; 1 Ihl' bL:~t onl' ) of sht:llac on 10l kd pi lb 01 Ih ' dry'd lar 101'
on caps uk, ) mak", a good ,nlcri ,' cO:ll ing LO
I. l'h' raw pianI IOps J re r"d11L','d IO a pulp
p rc:\'e Il l los ihrough \·Olnil ing. ril" la r wIi I
In ,I Waring blenda. a,iùill,'J lo O.I ~,;. aeid
kl',' P for sl'v,'ra l Yl·ar, .
wil hcitric a,·id. ht:all' d lo hoiling, sl r:linc:d ho l
'l'hL: thk k conù'n lr:lled liquid lllUSl b,
Ihro11gh parac hute: l11a[LTi ~1 1 and "q ll l:ol.'d dry.
acidillt'd prio r III L!\lr:lcl ion, sinn' c3rboll atl'
Rl'-,I '.:p ing. in :lL' idifiL' d boiling \Va ll' r :1 nd rL:-
iOI!> ll!icr krl' wilh , olu hi li ly of frù' 111,',cal in,'.
p r(~~ i n g ",iII r~lllovt: :IiJ1l0S1 :Iil Ira ec, or 3lka-
Expt' rimL'nts sho", tlu t Ih· ~ mint:-,: I r b onalc
laid. Di,cud lh l' pllip.
lo fr e:"':lJ1l inl' l'qui lit rlUJ1l in NaOH ~()Iulio n i,
2. Fr(èJ( Ih,' buds lO ru pll1rC th . L' 'lI s. tl ww, high ~no ll gh lO inll'ffac wilh Ihe e ffi c i~l1ry of
3L' idify 3S prL'viously no[e d , hea t IO boiling, cX lraCl io n. Ac idlllc3 tlO ll or th ~ pia n I wilh 2
0 / . citric ,I,' id pL'r 5 gal. lot bl'foft' cooking will
hOl-p l l: SS whu i' by pladng in a dOl h sac:k 3nd
t'r " 1l10S1 of [h .: alka loilb and ,\;:sl roy JII (ar-
11 si ng SOJ1lL' kind 01' lll a, hin(' likc a L'id"r prL':s
bOlla le by th ' li m,' thl.' Sol11 lion is COlh:~nl ral ­
l'or Ihe pr,' SSUfL' Ilcedcd lo squcezc ali Ihl:
liquid 0111. A ri cN or frui I sqUL'o t:r wo rks for cd . Ikn z,'n ' (OIlL' oL. /gal) may b~ u' ed ~, a
pr~sL'rvali\' c on ly if th<' liqu id is IO be' li sed l'o r
' 111all 31ll0 11n[s.
l.'Xlr:I c: llllll , h,xaml' 01' ils e:xlrl.'llll' loxkily .
3. Pressure cook the wilole pla nls, ac idifi,'d For l'Xl rJCl ioll . Ih ' lll~s~ : llint' mus I b" r,-
a, bdorc, al 20 Ibs. l'or 15 111 i nllle:~ lO di , ru pI IL'ascd :IS ;1 frl'l: base' : "xlr,1(l<.'d wi lh :1 ,OIYl' nt
[h" liss ues wi th litt I.: alkaloid lo". IIIH press to releas ' il fr0 111 Ihe pl.;nl ,ugar, a11(1 am ino

18
acitb in thé crude extrac t : and in turn. is t'X- to sC lll t: . POllr tlle benzene from lh.: sc lliing
trac tcd fro m th e so l \'\~nt by ,:olln :rs ion to the jllg into a clc:l11 jug, add :1 l'l' W drops o r IO j;
salt or an ac ido H,SO (2 ' ) and shake \Ve lI. T e ~l the;! bt:nzt:ne
To rcka,t' Illcsc3lin' J~ a t'r ' \? b3s~ . 'J usti( soÌuti;n with pH pape r to sc.: il' it is stili basit:o
sod~ is IIscd si nce Illcsc3 lin\? is excecdcd in Kt:cp titra ling t!le bènzc m: in this manner
ba~lc iTv bv l' W bascs Icss strong than l\aOH. l'Iith ac id \ln til Ih b..:nzcne b<:gills to turn
'l'hl' l'~ II~t-ic j, made carbona I<' frt'e by di,- ncutr,d. llli ' litration i' best ca rried out u~ing
sol\'illg il ill water to mak c a 50~; sol uti o n some;! kind or me hanical stirrer ~\leh a~ a
((, Ihs. :gal.). The ca rbonale sd tks out in ~ 4 ma gnet ie stirrer. Owr-acidity mcan \ bica rbon-
hom, :lI1d purè l' aOll solution is dccantcd. ah: Ill ust be u ed during recrystallJl.illion.
Kt! 'P :. \Va y fr0111 :l1r 3, It wi ll pic k up CO 2 and whieh in trod \l r<,s more;! contalll inall ts in th e
!'ix it a..; ca rb oll3Te. forlll al' minèra l salts which al''': a n\l i san~e .
'l'o t'V Ty four VOl lllllCS of the cooled t' X- A , mali :1I110u nt of mesca line left in th' b~n­
trae t co nl't'lltra lc add o ne l'olu lllt' 01' caustie Zl!n \!. ma kil g tlw solu tion slightly ba,ic: wi ll
solu ti oll . ~'Ii x in 3 large jllg and imlllediatcly not hurl at a li ,irn:c the nex t ste p is to relllrn
alld at bl, t two \'0IU111':\ 01' bClll..ene. Vt'nti la te til e lIscd b 'nzcnc lO thl! crude basi eX tr:Jet
the :Irea wt' 1I whc n using ben7.e n(; d Ut' lO lÌ1e solutioll for furth er l'xt raction . 1\0 Ile\\' ca us-
c'X trc111c ly p oiso ll ou ~ Ilatur e al' bt' nzcne fu 111 C S. tic is :1ddcd. "n d mixing i, dOlle card\dly 3'
Clo'l" th.: mOll th or' thl' .iUf! ti g.htl y a 11(1 inl'èrt bt' ror.:. The first cxtr:lct ykl d ~ abo ul 80~; of
smoo thl\' 50 timo or more to mix sol \'{: n t thc to t:!1 :1lbloids : the second, 16'-; : the lhird,
wil Ì1 t h~ extra,'l liqu o l. Do 110 1 sha kc, sincc .L~ '~; : an d th è fOllrth. k ,~ lh:m l '.; . "111 > crud e
thi, produ Ct'''; 3 thick emulsion wh ic h is :lll11o,t ex trac t is <:xhaustt:d an d may bé' discardcd
Im pos"bk to brt':l '. If 3n e111uIs ion dOl:!s l'or111 . art.:r four cx tra,t ions. bu i lhl.' lIsèd bcnl..:n,'
Ict , t:md an hou!' :lnd , ti r \'t::ry slo wly to hdp may b.. d l~t il 1t:d lo gl:! t rid of tht' v. JX" .md
bn:ak bubbks. If neccssary. adel morc ben zellc. gllm~.

Do Ilo t alloll' lhè 111 ix tllre to , tand 1110re th:lIl Th ~ l3yèr und",r th, be nzcne in th l! ac id
ì ur hou r ' if possibJc . ,ill ·c eau, tic ", iII hydro- ·x traetion cOllt:Jins mush}', impure a lbl o ids,
Iyze mesca lill t! ill tim<:. Whell p3rt 01' thè benzene 3nd water. Warrn th is g..:ntly. lIsing a
b<'llzc:n.: has layc rcll, draw InoSl o r il oif by fl a mcle. " heate l' 31ld good l't:nt ila lion. POllr
mt'an, 01' a prc'ssurc started ,;i phon (S~l' F igure ofr most of the scpararcd benzene anel cnp-
2). Colkct it in a bo tt i' :!Ild allo l\' any r~siduc ora te rhc Ia,t bit 01'1' OI'CI' a \Va l er LJath _ When
ali th~ :rys tals are di5soil'.:d, \If:lp th . l'c,,el
in ;J 10l\'eI lO in su lat<: il. Wh cll this slow cooli ng
has takc n th e tt' lll pt' ralurc to 3l11 bÌC'n t. piaCe;!
Ihe insu l:nion and 311 inlo :l rc.: frigc.: rator and
con tinue: cooling down lO 0°('. II' cryslals have
iormeLl , thc ma~sc~ an.: m ll~hc d up to llla kc
fillerillg ca. ier. -l1lc Lluchner vacuum filter
fU!lnel . almost :J Ilcccssi ly to the procedure, is
preparcd by wl'tti ng thc.: filter pape r alld
slIckin g it inTo pi ac e \Vith til e vaCUUlll a,pira-
[Or syslcm (se l! Figl1rl! 3). Fil t.:r the crystals
and wash thèm vlith ic-:: -w:Jtc.:r, then ael:! tone .
Rl.'lllol·": the mother liquor to 3 wann dry piace
S c l ti i n~ l ')-~-:r-r1l
Jug wh<.: r ' il m3y evapo ra te lO 3 lo '" vo lume . Re-
FIGURE 2
di~~oll" thl' dry crystal s in boiling wa ter 3nd

19
 cl c ju t doesn't produce good cryst al . This
is evaporated to dryness and aved for later.
Aspirator By this time the brown liquid from the very
first crystallization should be much rcduced in
volume. Heat this black liquid to dissolve solids
and add acetone cautiously with stirring. Use
IO times the volume in acetone. Cool fiJter
and wash with ace tone. Combine tlti with the
slightly impure solid abovc , dissolve in boiling
water, and charcoal filter it, recovering a cou-
pie of more small crops of crystals if po ible.
FinalIy the crystals wi lI begin to look fu nny,
although t hcy are clean. This is indica tive that
the less soluble me caline has a1most ali crys-
FIGURE 3 tallizcd ou t and the other alkaloids are start-
ing to erystallize. These a1kaloid are interest-
add one tsp. activa ted charcoal per 100 mi of ing and worth 'aving, but are non-hallueino-
solution. Preparc the filter sa me as above, buI genie and are slight1y poisonou . Many tailing
layer some acid-washed asbestos pulp over the may be saved lInd combined. Chromatography
paper to help seal it. Filter the sollition very will separate them and reeover more mescaline.
qllickly and very hot. Keep vacuum on as long Re-cxt raction from an alkaline solution may
as therc is cha rcoalliqu id in the fllnnel to pre- hel p ge t rid of a2504 exce es, This is the
vent leakage into the filtrate, Wash the fiI- complete puri/ication processo
ter with a small amounl of boiling watcr. TIIe final product is mesealine hemi-sulfate
Don't worry aboul diluting thc fi ltrate 100 2H2o. If pure mesca line, a clcar corrosive oil ,
mllch; if the sQlution is 100 conecntratcd it i5 de ired, the procedure i 5imple from th is
will not crystaUize right and po ibly thc filtcr point. Dissolve the pur~ hcmi-sulfate in a 10%
may clog up. Heat tlle ve sei with the solu- NaOH solution and e xlract with benzene.
tion in a dou ble boiler to re-d issolve any crys- Evapora tiOlI in vacuo gives pure mescaline,
tals formed prcmarurely. Crystallizc as be- but exposure to C02 in the air leads to the
fore. If (he solulion was treated proper1y , formatiOlI of mescaline hemicarbonate. Care-
white needles will grow in a cJear to light fui titration of the mescaline-benzene olu-
yellow molher Iiquor. The slower the erystal- tion with any desired acid and carcfu l, low
lization , the larger the needlcs. Crush the crys- evaporation of the resulting aqucous cxtraet
tal masses and fil ter, washing the crystals yields pure crystal' of the salts of that acid o
with ice-wa ter and then acetone . Dry the
producI briefly in a gen tic, warm ovcn (130"F)
and store in tightly closed bottlcs.
To gel a beller yield, one mu t go back and
pick up any loose ends wllere extra mc caline
migll t be. TIle first thing to do is evaporate
the last mother liquor taken from the pure
crystals, and get a eouple more crops out in BIBLIOGRAPHY
thi manncr. Each time the watcr solution is "Tbo Alkaloids", edited by R. H. F. Manske and H.L.
cooled to O·C, 3% mescalinc is left. Finally Holmes, pp. 313-334 on B-phenylethylamines by
a solution rcmai ns which is slightly brown or L. Reti.

20
Pe-y?o!!F.T~~~~CE~t
 ~IESCALl E SYNTH ESIS .~ I

~1 -:~~: t1 il h' .
th,' alkalulu founci in Lopho· is :tdeh:cl 3ml ho ili ng co n tilHll' d for 2 aùdi t ion al
phora wil lial11 sii cH't i has h<=l'n -anrd ura lly ho m" The' rl' ad ion l11ixtur<, i, lhl' n ,'oukd
ddìned :!I1d :y nthl.'sizl'O l'o r Ilearl}' 50 ytar,;. ,!l ld acidifi nl \\' ith d ilLi te HC I: th' prl'c ipi t:.l ll'd
TIH: fo ll o win g p ro~t' durl' gi l'l" OIW or t11l' lì r~ t tril11 l'1ho,y g:tll ic 3c id is tl lt 'r.:d with slIl' l io n
I11l'thoo, or ,y nth l',i, ,Iightly 1ll0d iriC'd, ~h n>' ami \~' ;r,hed \Veli wrt h -:old ""at 'r. TIH:' producI
ot ht'r routes te phenyk thy l,1I11inl' (kril :J tll," wh ir h ml' lts at I : 7- 160· i, ' L1 ftìcknt ly pu r '
a l'l' IKw;ihk, bu t this l';rri,i1 ioll giv's 3 mudl l'or nH),; t purposes, 50-52 !! i89-<)2' ; y i~ ld).
h,' t te'I' yil.'lJ, In mo, t pro ' 'dlll"':, th l' ,t art ing fUrl hn puri ri-: al ion i, ach :t:I'l'u by n:crys·
mal -riJI is thl' " un,' : .'. 4. :" tr ihydro:xy t ~lI i7:ltio n [rOm 2 !itt:rs of boil ing water wilh
bC:Il.oi,· :!t:id , mor.: l'o llmon ly know!I a, gallic 11l\.' li'" of d,' ~(> I ()r i Ling ~ 11<Ir.:oal: Ihl! l!l tra -
Jl' id. tl<J11 h,'lng l':!rri<'d aut in a sleam jackdcJ fun-
Ih:1. In I hi, way 41- 4 2 ~ oi l'olor k " nccd l 's
STEI' I 3. 4. 5, Tr im t' tho:x y Ben zo ic Acid Illl'iting at 16 7" i, o blaincd,
10lll' g o r \ :1 11503 I, adtkd IO a IO OOm l STEP l( - 3,4. 5 . Tr inlC'thoxy Benzoic
R13 111>1\ uJ1I taiil illg 500mll'old H:O wilh i\()g Chlorid e
C ;\1 k, o r I IO mi S()," ; '1)1 1 ;\ ,1011 J ll d 111 '
2'10 SO() g o ì tril11l'thoxy bl'll/oic acid , add
n,h , i, ligh lly stopPl· l':cl ;"I mi 'tirrL'd \\'it h a
':~ 5 1ll 1 fr,' , hl) di,t ill cd th iolly l chlo!id.: a nd
lI! aglll'l i-: qi rrl'r [o r IO millll tl" , I () th i, ,olu-
I l'a t thl' mi xturl' 1\1'0 ho ur, 111 :r wata b:ltll.
ti oll j, adlk d ra pidi)' SO g (U_~ MI III ok" or -I hl' mlx tu rl' ,.; di,ti lkd ul1<k'r r:dul'cd Plt: '-
g:r1lil' ,1,'i,1. C.;,r1k a,'i d III \aOII solu tion n, i-
"ur,' u.;in.' !!bss CO IlIl ' 'tiO Il, :It ali joinh, ::: I O
dill" qllll' kl wi lh frl'l' m:Y!!l'n to " b ro\\'11
g :; . ,I. .- tr iml' th o '\ y b,'nl.o! I 'hlomk boilillg
l'OmpOUllo , h' lle.: th' 1\ :"ISO," TIl.: Il:tsk io;
a t J.' ;'i0 ( 1X111 n ) <l r ' 0 1 t3ilh:d , Yil'ld I).,'; Ml'
r,,·,toP Il<' rl'd <] uk kl y Jlld sti rred unli l ali ot'
~ ~· S4u .
tht: ", Id is di s.;oh'l' d , S9 ): 16 7m l 01' uil11eth ~· 1
, ull'a re <0 ,71 moks l i, 1111.'11 addl'll ,md tl1<' STEP III 3. 4, :'i, Tr iI11Nh o.\ )'
Ila,k IS ,I irr,'d l'o r ': 0 lII ill Utl·';. h,'ing cook d by
Be!lI,alde lr yd e
IIIl':llh l' cold wal ~ r in onk r tha t Ih,' 1"l!lpl.'l":l-
tUl l' tino 1101 l'i,,' :lhol'l' 30 lO _,:,0, 1Di llll't hyl T Ir' l{ <h.:nl11und rl' du,·ti oll 01' :!l'id chlmi tl l'\
,u lra ll' funll" :11'<' \'l'ry toxil'.) OCl'asiol! :r lly Ih~ lo all!t:lr ydes i, "'l'd with thi, l'OlllpOlll!ll. lbillg
stoppn is r:ti"d to rl'k:IS\? any l)!'l·" l1 rt: . .. \ no cat al)' sl poisol!,
,ccon d portio n 01 X' ) mi di llh·th yl ' lI lfat' I~ ,' To prq ' ar thl' Pd -H:rS04 c:rt ~ll y ';(, n13ke a
t!il'1l :!(\ <kct ,md , t lrrin g l'lll11 illlll'd t'or IO m in- ,,,spl'll sion 0 1' I. ì P. dry palbdiulll ch lo ridl' in
!lI.:., lo ngl'i". Durill): tili, ad li tiol1 Ih,' Il' mJlcr:l- 100 m i 11 10 ,'on lainin g Imi ,0n ll<'l. "il"
hl' :.! t
tu rt' may ri\.: !O .:1()·4:;", Failli rt' o r th ' l 'Illpn - lI p OIl a st " a1 1l bath o r all o l\' toslanò l'or .;c\'a,,1
;.tur,' [O ris.' uuring t I! ' rl'açtion mdy 111,.1 11 :1 day;; ulltil a c,,":lr da rk rt:d SOl li li o ll is oh t:l ilh'd ,
lki:J ~ ' l' d rl'a;ti oll \l' h i ~h will b,'gin :t! mos l l'X - A 'Ol uli oll nt' 15 g :lI1h ycl lo lb \! .! 2S04 in
plo,i\ l'l y wlll'll r.:t1 1.\ is lJl:g li Il , ::001111 HJ O l' ad" 'd ill th~ co m.;l' 0 1' 5 min-
'I l!' fl:"k i,; Illl' n flt tl'cI IV !Il! :1 n:lll1x ~OI1 - Utl''; to a m.:chan ica ll y stirred SO IU l ioll or 2 1
d 'Ihl'r ,ln d thl' conl .:'n t, hoik d far '_ hou r, . g 133el: ' 211 20 il 200m I H:O a t 70· . I hl' pr..:-
In rdl'l' IO ~ :J pllni ry Ihc slll311 :'lllOull t or ~sta c'i pita ll' i, \Va,hl''' hy lk canlat ioll wilh hot
II'llIl'h I: prod u-:cd , ,I olu tioll 01' ~(y ',: \ :101-1 \\'a ter unlil lhc w:.lshing' do no r givc a prel' ip-
in :;Oml 11 20 I l ~ 1111 50~; Illadl' up te 3(1111) irare \\'irh l\ g:-J 03 , I h.: BaS04 i, tlwII Slb-

22
 pcnded in 300m l 1-120 containing I mi of plcted, the solli tion is poured into SOOml con
4 0~;é forllla ldehydc. Ths slI'pensio n is hca ted I-ICI mixed wirll sllfficient ice lo assure its
lo 80° and th~ solution of palladium ch loride presence tllrollghollt the slow addition and to
is added. The wdl-stirred mixturc is nellt raliz- main tain a t mpcrature of _10°. The precipi-
cd to li tmlls by the add i tion or I 1\ NaOH ta!ed 3, 4. 5, trimethoxy 13 n itrostyrl'nl' is
sollilion over il jleriud or I) lo 30 Illinlltes. separatcd by fi lt ratioll alld washing a nd may
Healing a mi stirring are continued for 20 min· bt: purified by c rystallization from 700ml a l-
lItt's aftèr a we:lkly alka linc reaclion has b":Cll cohol. The pale yel low plales which melt a l
0
obscrwd. Th~ gl'a)' prcl'ipi la k is fil l<!l'cd by 120. 12 1 a re obtained in a y ielel of approxi-
gelltlc- ~u tiOll a lld is dri~d in a d~si -cator O\'er matdy 78'.~· .
c:1lcium chlor ide. The dry catalyst ,'o nta ins STEP V - 3 . 4. 5- Tri methoxy
abollt 5'1;' paliadiuJl1.
B Ph enylet h y lamine
The hydrogc~n uSt'd mus t be frt'e from oxy·
gl'n . This is accolllplished by passing e1ectro- 4To 1000mi anllydrous ethl'f in a 2000m l
Iyli c hydrogen aver ;1 h('at('d coppe l' coi!. RH nask is added 57 gLiA I H4 . whilc sti rring
Drieritc suffices lo remov..: any 1-1 2 0. Sodiulll vigorously with a magnel ic stirrer. (It i' (l good
d is tilled xylene is put in th e rt'act ion vessel idea 10 lise il safety shield wh ile working with
wi t h the caty lst ami re n uxing i$ begun w ith a Li/\IH4.) Pl nce 72 g 3. 4, 5 trimc thoxy B
hydr ogell l1ush IO rt:lllOVC latent wal er vapor. nilrostyrene in t he thimblc 01' a Soxhlct èX-
2To thc s lurry or 1000rni boiling '\ylelle in tractor an el attach [he ex tractor to the flask
which has b,'cn slIspcndeci 60 g or Pd-I3:1S04 with a condenser above. Heat the flask until
catalyst. add 200 g 3. 4. - trim et hoxy bc nzoyl ethcr boils gently alle! tht: extractor cyc1cs.
chlorielc. This mix llIrc is hcatcd on an oil bath Altach a cold trap a nd a dry ing tube from the
0 top or tht' condenser to stop dher loss and
maintained at 150 a nel ;1 vigorous strcam of
hydrat ion. 5 Rctlll'X and react for about 59
1-1 2 i, inl rod l!cccI inlo Ihc boiling Soltllioll. Fit
hOllrs. watl'hing tlle eo ntents of thc extraclor.
the refJtlx l'onde ns~r witll a drying tube and
Th' operat ion I lay be interrup tc d at an y time
t'rom the re. bll bbk the gas throllgh a water
so llition. Continua lly t it ratt: the 1-1 CI be ing
as long as wa ter v~lpor does 1101 gel in. lf an·
other 50 lve nt. slic h as tctrahydrofuran or di·
f!ivCIl 01'1' un til no more is 'valved. This lakes
oxane can be fO ll nd which com bines solubili ty
l'rom 60-80 hours. '1hl' sollirion is fillered an d
and inertness to LiA I H 4 with solubility IO th e
prccipi la tt'd wi tll a Solli lion or ì\aIlS03.3 Tlle
nitroslyrene. the Soxhlet extrat: tor would be
a ldehyd c bisulfirè prècipitarc is filtercd a nd
unnecessa ry. ti me would be rCc!lIced t o 3bout
w<lshnl wi th erher. Thc compolllld is tkcom-
2 hours. anel tht: nit roslyr..:n ' coulelbeadded in
posed by boil ing with cxcess N:12C03 J nd the
,o lvcnt ~o l lition.
:1ldchydc is l'xt radc d wi tll e t hcr. Yield 120 g
A fte r t he r~~d Icl ion is complete ,'001 th,'
(70.(,) MP 74°.
tbsk in a n il'c-ba tll, stirring vigorously, a nd
STEP I V - 3 . 4 . 5· Tr imet h ox)' ca llti ollsly hydrolyz<.: the co nlcnts by adding
J3.N itrostyre ne c h i p ~ or iC' thro Igh the condenser (c'\traclor
A sollit ion of 40ml nitrometh,lllt' and 100 removed l. When the reaction ceases . allow to
g 3. 4. 5 rrimcthoxy bt'nzaldt'hydc in 200ml si t l'or 2 Ilours. Add 500 mi I 0~1c. NaOI I and re-
a!coho l is cookd to 0° ;lIld wll ile il is stirrcd move the t'tller solutioll. Extract 3 t im 's with
me Lilanica lly. l h ne is inlroduced a solu tion of 2N H2S04 using a l11agnl' tic stirrcr. At pH 7
45 g pure KOIl iII 4511l11l20 alld 90mlmcth- ( 011 pH paperI. pour o ff Ihe so lven t :lI1d rc-
anol (lt the ratt' or abou r o n~' drop per second o c ryst allize III", m..:scaline hcmi-sulfate di-hy-
c;}r ' beillg ta ken that the temperature does noI drate rro m boi ling wat ~ r. Yield . 74-86 ~( i\IP
ri~e . 15 millutcs aft'r the a ddi l ion is com- 183·186°.

23
 REACTIONS

S ' ln in ~ wlth I ono g I)Jlli ...· .H.' id . ..·.I.. h ~ Id ll ~1 \l' 1I .J~ rq,HJllcJ In Ih.: J,!~·r .!lI.h.'

o
'';
0 11
EJ

Il 1000" 1"11 J CII, 119" r.

I I~ h:

Il

() li
+
/ Il,
( I 70,(" I

+o'.::::: ~:""'_-I.-": 'I-1-I1-\;:'"·\l--''-·'-l~:' ' ' ~

Cl ~ n
CH, o ( Il)
Il H
Il Il \ /
:-. x SO.. -x
/ \
•
+
I . 1111 .. ~
Il CII

III Il
III Il
I è/!,O
lICI!
1

I~ I( Ul.,:> k, I il~
l'. thcr
O/! o~ +
o h- o
( il, O ( H.

BIIlLlOC;RAPlty
Gi lma !l, Il . ""Ò
A. I I. lliatt Orgdll /C S.I'lIrill'su, p . 5:n.
Slo l (;! 3!ld Syz!\a. J. l'ra}..:,;. ('11"/11 . 13 7. 339 \ 1"33 1.
~i O'\l· ttig. E . d THl R . Mozingo.Orga ',!'C 1<c..'Cc..'!IUNL Vo1.
IV , (,h~plèr 7. p. 362.
G3ylord. Rr'(/u (' U() " w:l!: rompit' \, .\le.',1.' '(va'ride'L p.
764.
Il~!ln i.ngl on . F . ;!nd R . D, \ Iorln . Journal of lh e Am~ri ­
can ChcmicJ I ·o clcty. 73.13 53.

24
 MESCA LI NE SY NTH ESIS =2

-I his ml!!hod 01' synthesis is illl;l u d~d be- ove r sodium sulfatc, are frecd of ether amI the
ca usI.' it is co mm o nly uscd and is a littk residue d istilled: b.p. 135-13 7° (0.25111111):
casier Ihan the first one. Thc advJntage in t he yield 14.7 g (ì3';(.). Again , some 3, 4, 5. tri-
fir st sYll t hesis is an overal! yiel d of nl!arly 45';. , me th ox}' b~nzoic <Icid may be rccovcr<.'d from
whik this proce dure nels on ly abou t 5% the- thl:! ex Ir;l(; Iion residue.
orclical yie ld.
STEP IV - 3, 4. 5- Trimethox y Benzyl
STE P I - 3 , 4 , 5- Trime thoxy Bell zo ic Acid Ch loride
lJ~(' t hl: proce dure for Step I , Syn t tll;,is # I . ;\ mixlun: of 25 g o f 3, 4 . S, Irimet hoxy
STH Il Melh yl Ester of 3, 4 , 5- bCllZy l <.t lcohol an d 125 mi 01' ice-cold con
T rimethox y Benzoi c Add hydroc hl o ric acid is shaken vigorously un til il
homogenous solu lion is ob tain<.'d. I li a fcw
To a sollition prcparcd from 100 gol' 3, 4. minutes a lorbid ily d.:vdops , followt'd by a
S, lrimd hoxy benzoic acid (0.4 7 "l ole) . 20 g heavy precip ita tion of gUlllmy prod uct. After
sodium hydrox idt: . 55 g of sod iu m carbonatc four hom, and dilut ioll wi lh 100 mi of i' <:!-
and 300m l 01' wakr is add.:d, wi lh ~ t irring, wate r, the aqueolls layer is dccanted alld ex-
94 mi 01' dim<'lhyl sulf;llc (0.9 4 /'.'1o!..> l during tra tt'd wit h thrtt: 50 mI portions 01' benzl:nc.
thl: l~ OurSe: or 20 minlllcs. The reaction m ix- T h<.'n t he gummy o rganic residu<.' is di ssolved
ture is rl'flllxcd for on.: h:iIf hour. Thc' crlld" in the combined benzene ex tracts. The ben-
e,;ter U;5 g or 6 1'·; y icld) pre:c ipil atcs from zene sollllion is WJshcd with watcr :lJld dncd
t h ~ coiti mixtllJ't·. Frolli the filtrall'. 3R g of 01' .r $Odiul11 -ul fate: . Thc benz('ne sol ution is
s l ar t in ~ nu te"rial is rc.'cowred upon a,idifi- thl:!n Irans ferred lO 3 di~ t i ll alion fl:Jsk and t he:
ca li !l with Jilll tc hyd ro-:hlori, aci do The eSler b~I1It! l1 e is re ln oveò lI nder dimi nished pres-
i~ furt lh:r purifil' d by solutio n in Ihe mini- ~lIr<.:. 'l'hl' r,d St:I11I - ~o l id r.:s idlle is slispend.:d
mlll11 allloun t o f mcthano l and trc.'Jtmenl wit h in 3 sma ll :Ullollnt 01' iCt:-co ld et her ami filt 'r.:d
nonlt:. Lsually it is nl.'cessary lO repl'at Ihis th rollgh 3 dli llcd funn cl. Tllc crystalline prod-
In.:atnH:nt IO obtaina colorless crvslallinc prod- UC! In:!)' be further purified, anò art.:r fom
UC! th:tt !Ilells al 80-82 ' C. . r<.'CTyslallizations from benz 'ne. colo rkss nl:<>
dies art! obw in.:d; "IP 60-62°. This prod\ et
STEP III - 3. 4 . 5- r rimcth oxy Bcnzyl
shollid noI be stored vcry long as it may hy-
Alcohol
drolyze lO a sligh t cx ten!.
l'o a su,p<': !ls!on of 4 .6 g (0.1 ~ "'Io le) of
lit hiulll ~ll1lllinl1m hydride in 200ml anhy- STEP V - 3 . 4 , 5- T rim eth ox y
d rou s .:th~r is add ed , in t h~ com;e of 30 min- Pheny lace tonitr ile
u k s. ;I solUlion of 2~.(' g (0 .1 "l ok ) of th .: A mix tu re of 9 g of potassium eyaniòe in
Bl\:tltyl eskr of 3 , 4 . 5, trim.:thoxy benzoic 35 mi of waler and 60 mI mdha nol and 9.7 g
~ç i d in 300ml 01' dry et he r. Thc soild wh ich of J, 4. S, trimcthoxy bc nzyl chloride is heat-
form is care: fully dcc ompo l'd. first wit h 50 cd fo r tcn minut.:s al 90°. Tht.: o;o lvenls are
mi 01' ie' wala. cau liously added in small por- pa r t ially removed under diminished pressm e,
lio us. After d<.:<.: an la lion ()j' lh <.: I!ther, 250 mi Thc n~ s id ll e is iht:n l!X Irack d \Vith 90 mI of
of ict-cold 10<:'r sulfurie acid i, add t.:d. The ether in th rcc portions. The combin cd ex-
product is ex tracted wi t h 150 mi of elh<.'r. lrads are wa,hcd wi th water and dried ovcr
T h ~ cOJllb i n~d ' (ha ex trac!. afkr d rying sodiu ll1 ~u lfak . Ait er n.: 11\ 0\ 31 or the drying

25
;J =;~nt. 111<:' ,'lh ' r "olul ion i, W;lfIlh:d on ;] ,lt';]1ll \Valer IS dr oppl'd ill (;J rl'ful ly, I hen a mixllIr,'
balh ;md Ih e 'Iher is r ~lllo\'ec1 wil h ;] .;r r,' 3m oI' IO g of 'lIlfllrtC :te' id il1 40 mi 01' i(T-\\'<1 ll' r b
or :Iil, On ,hillin=; , Ih,' rt',idllt: yi,l(b , 'ak-likt: ,Id(k d ,Il a moda,II ' r:lIl', fht' :lqtll'OlI ];IYl'r
\.'ri ,1:lk Kt:nY'I,tllizalion l'rom l'lhn t:i\'t:s rC'l'- is ,'p:lrall'd an d lrt::!lc'd \\ilh l'OIl sod illm hy-
1~llgu l Jr pr ill,': \'i,'ld, 2,5 g I 27': I : :-'11' 76-77' Jro:-.i(k, 'l' hl' broll'n oil i, l':-.lr3l'1l'd wilh !llrl'l'
portion~ 01' ,~O mi l'a('h of b('1l7t'Ill' , T Ill' cOIll -

STEI' VI \l e,c:tl illl' bint'c1 bt' nz,'llt' l':I, lr:h': h ;,rl' lilr:lkd lO nell lr:t1-
Ily wilh IO' ; ,u lfur k Jc id, r h ... aqul'ou'i Iay,'r
In 1:'011\ 1 1'( ,!I1hy d rom l' I h ,'l' i, ~lI,pc' lllkd i< tilt nt'J lilrùugh ,11:Irt'oal. hl':tll'd, :tlld ,ookd
lU i: g f lilhium :tlullli lli u ll l hyd rid.: p' l\ldl'r. ,101', I ~ IO yit:ld ,o lork" Ile: 'di 'S \\'Ìll ch ~Orll'11
\\ ilh ,Iirrillg, 2,0 g or 3, 4, 5, Iri nh'lho'\y ,I I 1-;: : 0 alld 111\:11 a l I ~2° ,

pill' l1~ la,'c'lol1ilrik in 1:'0 1Il! or :ll1 h ~' dro u'

dlll'r IV,lS adI"' '' dlllin~ lht: t'OUI"'" or IS Iilllì- \1. U. l , au, J \ ~lIl n.li ul tht:' ,\ r!l ::ri,::.t ll rhl· ~ l i ...1i c.; n"il--
\11\:" .. \fk r 15 minutc" 'lirrt ng, IO IIll of in '- :y ì.; , ~ ·,q5- ."'·l <J (, .

,\ I I-.SC\ Ll1\I: SYJ\ TH ES IS - ;: I 8: " 2 CO \IBI J\I::D

All Inl erillediale Slep
1\ good lllClhod using 11l<: bés h~ lv<:' of I hi, rl'agl' II1 is <: a ,i )~ ' prC] arl'd by addi ng a n
bll lh pron:dur,', im'o ll"-" {h<: t'ir.;r four sreps of ",:-.ç<:" or' ,Oli ,1I11mOlli:, tu:j Cor m,di ll , ,,11I 1101l
rhl' sccond mcthod , w,in!! lhl' Soml11<:kr r<:~c­ :lI1d l'"apor:liill l: Ihc' 'lliu lilln lO Ob" lill Ilt l'
t io n tù obl ain t h<: :t1J<:hyJ<: , :llId fi ll l ~hing ,olitl hl.'x;II :I"th~ k ll t' tl' tral11illc', Rdlu:-. Ihis
Wil il l hc fir'l rllctll\ld ; q<: p ~ f(lur ~ nd fil'<:, mi'\l !! rl' l'or 0 11' hOllr ,ll1 d plllif~ ,h,' ,t1Jdl~ d '
:1< in SI,'P II I, ' yllt h ~", ;: I, Yi,' ld 70-.\0' : :
Inlt'rtlwcli:ll C' SI('p - J, ~ , )- rril11clho:-.~ 70 g, Rc' l'Ol'c' r :lny 1I IH l' ,! çl~ I 3, -l, 5, Irtnl\:lh-
BClll:lld('h~ de Il;;}' :lkol10 1 <li' ()\ c'r-o:-.idi/t'li :l CI<l lI sin ~ k l' !t-
niqllt', :I> illl'lIrilìç,dioll or lÌl osc In ll'rIll,<llal" ,
l'o:1 'Olll l iull I \ t' 100 g 3, 4, ) , lri ll h'lho xy !l 1!ll JOGR,.\P1JY
I ,hlùrid,' in 5UO mi, 1,0' ; aq :l<:o,,, clha n-
bl" I /.~ f i\.!s(' : ~ nd F l t::"II..' r. Or~ l1 : (: Ch~1I1 1 ,try. 3rd l-dH 10 Il . p.
o!. i, :I\ h kd ,'O g o r h,':-' :lllld hyil'Il,'klr:'llIill,', h -:;
o Oell,
11 / .
c

~
+
II I
c ile i
I

CI
I

:'\0. I :lJld ~O . 2
Il c'\JI::C thy (.."ne'te :r:J :nir.C'

27
 rS ILOCYU!:"l CULTURE

T h~ pllrpos~ of t h c~ c' instrUl' liollS i, lo pro - s!antcd ,uriacc in the tubI.'. Innoè'u late th e:
vi(k Ih.: tktail, of produçj ng p, illlCybin l'rom ,l:tll ts wi th thc eultl11'es l'ro m the Pctn d ishcs,
3 nalur ~1 sourù' . Tlw trad iliona l Illll,lt roOIll' laki ng L'afe' to k~\.'p <.'\,çry thing fr e" from cx-
Jrc diffil'lli t to gro\'." , but lh l" fung:ll lllyL"diJ tnll:lIcollta mina tion. Thl:! light ly t:J ppcd tubcs
or tltr"Jd-lik" port ions of lile' ,allle orgalli,m an: ,tor,<I at l'OO1!l tt'mpna tu l'e: lIn til a mycc:-
IIl:1!' he grown in n li tllr.:. prodll -: ing èOIl,idn- li~1 Ill a l has !!l'OW Il . SrrL' w Ilw t'ap' tight ami
ab k l',ilocyhin. , tor ... 111 a rdrig~r,ltor. Th t'st' \V iII k~,'p abOlii il
Il is illl pOrt:lI1t in working witlt fUllgi to us,' ycar bcforc' th.:)' will Ih:~ cd rt'c ull llrilig.
pllre' c:lIlt urc' I,'r hnlqu . to pn""'nt tll<: \'igorolls Thc main ClI ll ure lllediull1 is a liq uid , prc-
wi ld 1I1111.!, takin g m' ,T thl' , 10 \\l'r gro wll1g p:lr.:d : I ~c ordi ng lO formu lae: It, ted belo\\'.
Ibiloc' yl' ,' rI111gu,. l'ur... cu lturl' tn'l lIliq ue is Cul t li re' ja rs m:\ y èOlhist o r' variom-silxd m:lson
trO::ltl"J in dt'l:li l in :111)' good mic robiologic'a l j:H~ witll -:o\' \.'r, m3de t'rom hea \'y-g:1 uge :Illlmi-
manu;!!. Ikt tn yct. finti ,0Illc' 011l' who has h:1d 11I11ll (oi !. In as illudI ~I , ll1çdi~ arc pn:p ared IO
b:lclc'r1o logl l':1i tr:tilllng to h"lp yOll ka rn how clil ture Psi/ucybc m)'cc1 i3 to tll" c:>.ti nc tion 01'
to tr:l1bkr L'ldtur\.', Wllh a n inn o\.·ul:ttin g loo Jl . ali othcr org,lIlisms, it is ne cessar}' lO stcriIize
Thc psilocybl' 1'1111);1" Illus t b ~ pur\;'-n dturl'd the cult ure p l'S wi rh th e m, diu!ll in thClll,
prior IO an)' o tl1<'1' opl·l'a tions. ~ l akc' :1 sll:r ik S ter il iza tion is bes t accomp lished by pl ac ing
\\\ 11(' 1' ",l u tioll or Ih... spo rc dllq :md pl:itL' il the cO\'l:red jars (no more than lul f full uf
alli in dilu lion, on potato d ... xlros,' y ... as l :Ig:lr Illedilllll) imo a eann ing prc:s<;ure cooker co n-
in l'dI'i di,la:s. A(ta gro win g s ~ \' cra l days t~in i ng a li u lc water . .'\ temperature or 250' F
SOIll" o r th ... plak, ,holl lù ,hall' ,igns or th ", is Illosr casilr Illain tain ed if thc prt: ssu re cooke r
whil<: Illy\.·... li ~1 Ill:lts or Ihl! psiloc) b... r'lI ngu, . 11:15 :I ga llge giving tc:mpcratures :!.t diifcrcnr
Olw ioll ' wil d 1llold s m usI hl' di'ca rù 'ù :Imi lile pressurcs. Altcr 15 IO 20 mimm:s, cu t oif th e
-"k-:t-'ù c·u IturI.' growl hs Illay be tes le: ù b~ hl'ilt. but keep the cooker scakd. 35 suddèn
r ~èu l t ll ring in PD Y brotlt .md tcst ing:l I1lè lh :l- luss u r pressure will CJlIse the mcdiII m to ho il
noi extràct of rhe ìungus with th, Kdkr-Re:' O\·cr. I f the te mperatu re goes rou high o r
agel1t (see note l>cIolI'). cooki ng is too lo ng, some (lI t hl' sug:lrS will
~I ak\.' aga r sla llls for stori ng cu lture, I )' lì l- lx:gin lO carill el izc. T his reacti on rènde rs thc
lin g (, ilh.: h hy '/, illch ' Cf t' w cap tub\.'s Oll e:- mcdiu m u nlir fur growing the fungus sin ce
th ird flili of 1l!elteù rDY ~tgar. AlIto,'lavt' :md caralll el sl uws gro wrh .
Ic i ~ ool at an 3ngk so the g\.' lkd Jg<l r ma ke, a

29
 J\,\ EO IA FOR.M ULAI-:
Po t ato Dc x trosc Yca, t "g:lr

W;lsh 250 gr~m, pot atoe, (do no t pccl),

Slice 1/8 inch l h ick,
Wash wnh tap w atel' u nti l thc \\':lter i~ c1ear
Dr:li n , ri nse w ah di sri llcd \\':Ht:r
(ol'cr Il'il h d ist illcd \l'a ter :tnd <:ook U Il l iI tender
Dr;lin lilJuid rhro\lgh nan ne! clorh or ,cvera l rhi d: m:sscs 01' ehec'ecloth in te ;1 ilask or pr
l{i!hC pot.ltoes once or tw ice \l' il h a Iiltlc J i,tilIe J \l'at..:r
Ke cp Iitju iJ amI thm\\' pot:ltoes a\\' a~ ' - add c:nollgh Ji'lilIcd W.lt C"r te !l13ke up or.C lite r
of IitjlliJ
I3r ing IitjuiJ to 'I boiI :Ind ;\dd:
15 gr;lIns 0 1' agar - st ir lImi l Jissoh'nl (\l':ltch C:lrdul1y or
it \l'iII bo il ol'cr - bc,t te u sc :In open st;lin le:s' stccl pan)
1() gr:lms (l I' dcxtrose
l , 5 gr~l11s of l'Cast l'X tracr

Whil e Iiquid is hor. disu ibllte in to desired contaillcrs

:\ uroclal'C l'or J 5 m inute , al 2500 l, (about 15 los, pre~surd

PDY brorh i ~ nude in the S:1I11e W ,lY o mittin i! thl' :tga r

ry" gralll mcdiu lll:

for l, l p int ja rs : Not e: thc 2T:li n med ium m :w '<:<: 111 to
50 gra m , rye gr :! in (\l'hole) l)l' :; bit drl' H tim es: il' so. ,1
HO mI. \l'ater rew mI. oi' ster ile: I\';!ler m:l l' be
added . '
1 g r:tlll c h :d k (Cllc iuJ11 orl.1011:1lc) Th e fle mcdi ul1l i, aIso lI sed a, :1
" 'p al\:n " l'or illnoc ul:lt io!l o f ho rse
fur plllt prs: IIlall Ul'l' compos .15 is done in
100 g ra ms rr e gr:lin commnc ial m u shroo m c u iture,
.\ \(:. th od~ for l!fll\\ t h 0 1' Ps~:! ()q'bl!
J 60 mi. I\':lter
011 compos t lì .!I'c bccn \\,òrk c(!
2 g rams cblk our, bur lTtjui n: :tcce" lO :l com-
mercia i sourct' of compost, o r
for qU3rt j:ll's: kno\\'-ho\\' 0 1' prl:p:lri ng ~11l :tl J
225 gr;lJllS n 'l' gl'a in ;lI1H.>unrs of cOJnpO~L !'::., n h '.\j;Cil N.1
do cs nor iruir 011 com post, b Ul
275 m i. \\':lter 1 ).\. '1 ! j;(· H.\ ,;.\ \\' i 1.
4 gr:1ms cÌlà lk

30
 Afll:r prcparation :lI1d sll:rilization. kecp tht powdcrce! ane! exrracted rhree t imes with
media at room t.::mpcratllrc for thre.: days mc!hanol and thc !11ethanol carcfully evapor-
without op\.!ning, 3S a cht'ck lo see if tile ated. 1\ hair dryer does this ni celv. but t he
stailiz<ltio n tcchniquc was cfft'ctivc . Any fumes from merhanol are rerri bly . poisonolls
growth or sCll mllliness indicatt's lInwanted ane! thc arca must be well vent ilated. Take
groVltl! and that lllediuIll !11wt be discarded. C:lre to relllove ali of the poisonous solvent
These large cont:lin\.!rs 01' broth may now from the psilocybin residue.
be innoclIla!ed carefully with loops 01' whiti~h Practi ce, with tho.: hdp 01' a competen t
m)'ccl ia !akcn from th c pure stock cul tllrcs. bactaiologist , will improvc yiclds. Il' possiblc,
using pure eul1ure tcchn iquc . Kccp co\'cred ha ve a n expert in mycology isolate the pure
and in cuball: al 70·7s~r l'or IO-I~ lby. psilocybc fungi from thc dried mushrooms.
Temperature is important as thc fungus pro- Psilocybe cubellsis grows and fruits rcadily
duce ' psilocybin poorly at higher telllpcra- 011 the potato dextrose ye ast (PDY) agar or 011
turcs and grows poorly al lowcr tempCr3!l1res. st.:rilized grain suc h as ry.:: Psi/coybe mex;-
Ideally. han 'esting is done fOUT days aftcr ali calla frui ts on ly on PDY aga r.
tlle sugar in thl! !11cdiu!11 has I l'cn uscd by Se\' thc U.S. Pharmawpoeia l'or liti? Kdkr-
lhe fungus . 'l'hi, may be followcd wit h th c use Rea gen t. a 'olution 01' ferric ehloridc in glacial
of a simpI.: saceharilllcter. if desire d. Otha- acetie acid usetl as a genc;ral tesI for alkaloids.
wisc. trial and error will establish the opli- ( . 0 1 specific l'or psilocybin.)
!11um incubation time which will produce lhe For illust rati ons of lhe fruiting bodics (car-
bcs! yiclds. phophor.:s) 01' P~ilo<.:ybe mcxie:lIla se,' CompI.
Thc cullu re conlains a mal of fibrous Rend. Acad. Sci . 246: 1346-13 5 l ( 1958).
!11ycelia at thl' en d o f lh~ growth paiod. For the .:xtrael ion method see Experimcn-
'o !11ushrooms or carpophores are produccd. tia 14: 107 (1958).
bu t these aro;: Ilol cs~\.!ntial to psilocybin pro-
du cti ol1 sinec lh .:: myccli a contain an equa l
BlI3LIOGRAl'HY
pcreentage. ri ltf.:r llu: Illediulll th rough a flan -
Co m p:. Rend. t\c .ld~ Sci . .2:1(i_: 1346-1351 (1958)
nel c1olh. collee! thc mattcd myc lia from
r~xJ}~nm e nt.!l!.l:L 107 ( 1951»
the eloth and dry it in a dry ingoven al less than ~!crriott. Merlo:. "How To Grow Psilocy bc Mush -
200~ F. /\ ki tchclI o\'cn may be used if the door rooms"
is kept partly ajar ane! thl: t<:mp.:ralurc IS Hrim . Rogrr ct W3~o n. R. C o rdon. !-A:,_Cha nlQi 'non,
wa tchcd closely. The myce lium residue is Il3l1ucin og ~M'; Du Mc xigur.

31
 SYNTHES IS OF PSILOCY~

Inlrou uclio n
This ~ynlhl.!,is is (h;~igncd lo produce psilo- di ssolVe'd in w;lter :lI1d dropp<!d in wiliil: the
cy n l'rom obtainable IIlJtcrials, but is v.:ry wholc Ih ing is coo!.:d in :In iCl·-ba th for two
long and involves many sleps JS a consequence . hour,. ·1hl! Il holt' rC:l<·l ion may -:oll\'l'nicntly
b~ carricd Oll t ili a gallon jug il' can: i, iak<"n
STEP I
lO prOlcc t thl" glJss from therlll ~1 sho('k. R ~act
6-nitro ortho-loluidinC' is prep;m:d hy ri.:duc- thl! so lll ti on ol'<!rnigh t in a rl.!fl ig.:ra tor to 1.lkc
lio n of 3n ammoniacal-alcohol sollltion of 2, 6- ca re of in solublt: r,':tc t3nh. To thl' j llg con-
dinitro loluene us ing hydrogl.! n ,llltìde or t,lining the lì ltl!r·d c' ool,'cl solut ion add ~167
Jmmonium su lfìdc. mi waln wilh ~:;O mi COli ,u lfuri<' :!cid alld
Hydrogen sulfidc is a dcadly. foul-smc ll ing W;lJ"Jl1 in J 13rgè k<"tti<: full o f \V:lf!n lI a kr
gas whit:h lllust !J..: handkd out of do o rs on a gradu;d ly brollgh l IO :1 boil \V hik th,· jug is in
wiml )" day. This rcagcn I may be' purchascd as il. Art.:r lIitroge n b1lbbl,·, C C::IS C lo be cvoh·cd.
a cOlll prcsscd eylinder gas or may be gCl1eral- lì ll the jug n<?3rly lO Ihe top an d sk im any r~,i­
l.!d by ae ti on ofacid 011 ferrou s su lfid· or wa kr d1le from Ih~ surt"acc. Cool Ihe mi"\ llIrc slo\\"-
on alullli num sulfidc. Ammo niull1 sultì(h; so- 0
Iy lO near 0 JnJ filt,'r Ih' l:f)"q:rllinc !lltro-
lut iol1 is much sarer and casie.:r to llSC and is nc;,ol l'rom thc solution. Etlwr ,·x IrJetion of
produced in thc rcac lion anyw:!y. ,'vel1 il' th(· the solut ion \Vili yi,·ld ;llIo th,-r gr:llll of prod-
gas is w,cd . uet. Yield. 22.2 g.
20 g of 2, 6-dinitro rolucnc is ll1ix cd with
60 mi of 93% ct hanol and 50 mi of conccn- STEP II I
rratcd ammonium hydroxide. Thc ll1 ix wrc is
w:lrmcd and stirrcd whi lc hydrogen sul fide is Dissoh·c 7 7 g (,- nitro ort ho ,' rcsol in a so-
bubblcd through thc solu t io n for onc hou r. I f lurion of 20 g ,0JiUIll h}"dro\id,' in 200 mi
amll1on iull1 sul fidc is addccl, thc ammonium watcr in J roundbotlolll Ila<k. A Ir:lc· 01' so-
hydrox ide is nor necessar)", but lhe sulfide diul1l su lfil(" lI"i ll rCI11OI'C :Iny dissoll"ed o"\ ygl'n
solutiol1 must be added dropwise over thc which mighl ()""idizc tlw ,odilllll L"rovi. Con-
period of an hour. "l'h e solut io l1 is transfcr- Irolling Ilw tempn:l!urt: with ali i('e-b:llh. add
red to a casserolc and thc alcohol cvapor:lted. ca uti oll,ly (,3 g (4 7.:-\ mi) o f ('old di11lethyl
The residue is acidificcl wirh HCl and is ex- sul f:lt.:. m:lking 'lIrl! that the CJ"e,ol i, C011l-
rractecl with thar hor acid ic solution. the pktcly di:>soh'cd fi rst. EXlend Ih,· il ddit ion
toluidine bcing only p:mly solublc in cool lO the pl!fiod of o ne homo vigorously swirling
water. Filter thc sol ut io n cool :md make ba;,i c th l' ('on (ents after e:lch :Iddilion. Al' t l.!!" tile.:
with ammonium hydrox ide. filtcr and w:lsh addilion is C011lpklc . co ntinu . swirling whi1c
with water; rccrystalliz3tion is not neccss:uy. Ih e Ila'" wann, up to rOOl1l klllperalllre and
w~rll1 tile Il;bk fmth'T lO 100 in a wakr b:l lh
0
Thc basc mclts al 91.5°; yicld, 96%.
far a n hour . The product sc:par:rlt's 011 1 as a
STEP Il
dark oil ili thc boltom which may hl.: \I·;hlr ' d
25 g of 6-nitro orlho toluid ine is dis"oh ed wi th hot \l'a ta. Coni <lnd e'\ Iraet !he duk oil
in :l mixturc 01' SO mi ('on ,ulluric 3eld in wilh benlt! lIe or ~ th<!r. Ory the solution over
800 mi of wa ler. 12.5 g of sodilllll nilrite is allhydr oll~ sod ill lll ,u lt":ltl·.

32
STH IV in 200 mi wakr) is add ed lo tht: tc:ddish-
bro wn, :11kaline solut ion , Reducl ion is instan-
2-nit ro (,-mcthoxy to luc-ne is converteò to talleollS 3nd the black mix tllrc is hea ted o n a
2-n itro (,-mcthox y phcllyl pyrllvic ac id by re- wat er-b:lth for hall' ;In hO ll[ with frcqll,' n l
ac tion in po tassi ulll et hylate an d dil'thy oxa- ,haking , 3nd ihl~ n gt'nt ly boi k d l'or lhe S,lIl\ t!
Ia [(.: , Icngt h oi time: , Afta <.:ooling, thc bbçk sllldge
Pota~sium metal (7,8 g) is shaken under of fertic hy drox idt.' is 1iI1 er\!d 01'1' LI ,i n,!,! SO Ill C
xdenc at 100· until it is rc:du '..:d IO il rint' lilter :Iid such as Cel i tl~ orasbcstos pulp lO kcc p
s~spc n sio n whic h rc adi ly sc ttlt:s as t he liquid the iilter from b~<':Olllillg stoppcd II jl with thc
cools, t\ ftn tht.: xvlcn e has been dt.:ca nted. the slilll\' black precipitate, \\'ash thc pn:cip itatc
metal is lI'ashccl ~wice with :lnhyclrous crher with' dilllt, hol ;JlTlIllollia Uil lii a portioll 01'
(170 g or 238 mi ), lt:aving tht.: last port ion on tht.' ìil tr:lte is no longcr .:Iolldy wl1cn aci diticd
thc powdcn.:d meta!. l'his operation is \'cr)' wi t h Il CI , Co ncen tra !e the filtrate ncarl: to
dan gc:rolls duc to tht.: reaetive na turc of po tas- dryncss, 3cidify with 1-1 CI and ext ra,'t with
si u~ mctal and cven contac t with damI' air 3c't0!1e, E\'apor:ltc the acdont.', dissoh'c th e
is likcly to star! a fire, I\ bsolute efha nol is rl'sidllC in ;! sma ll pOrlion 01' con :ll11llloll ia
call1io~sly added to thc ether-potassillm slu r ry ami re-acidi !'y wi lh ileI. 'I h.: (,-l11c thox y ind ole
care bc ing taken no t to add so much at once 2-c<Jrboxylic 3c id ,~pa ra ll's ou l 3S a dirt y
thar the ether buils too vigoruusly, After \l' hitt, sandy pr\!cipi tat e , whidl is colkcted
standing o ne-half hOllr, t hc liq uid j, fi lkd witl! ;lI1d dri ~d at 100·, 1\klting point ~:<5 ° ,
a crystallinc precipi tate of potassi ulll et hylate,
Oicthyl OX:l!ate( 2 9,2 g or 2 7ml ) is noli' ad clecl,
STEP VI
The solid ethoxide disso lv es lO a c1ear orangc
sol m io n with the production of suffic iellt heat 3 gralllS 6-methoxv in do le 2-ca rboxyl ic acid
to cause thc cther lO bo i!. Tu this clea r solu- is d:col1lp osing by ill.:at in g at H5-25(tF for
tion is added 12,5 g of 2-nitro 6- mcth oxy on(' hOll r and th c indole distillcd at 181-IR3"
toltle ne, and thc reae tion mixturc immedi- :lt 24 111m Ilg, i\ ye ll ow cry~tallinl: mass collc<.:ts
atel v nnns rc d, t\iter [hi s h:L, bcen gentI>' in th e rcc èiIT r :lI1d is po\\'dl'rl'd 3nd wa rll1('d
hea ~cd undc r ren ux al 35-3R' for 18 hou rs, with di llllc potassium carbon:lll.' to r,'mQ\'('
the po t;lssium derivative scp:lratcs as a dark lI IlCh;lI1g~d ac id , Filt.:r ;Ind \Vas h \\'ith J illl tc
rcd, r:lther g11ml1ly precipitate. wh ich i~ ex- pot,lssilll11 c:l rhollatl' :In d thcl1 W:lt 'r, savi ng
t Llcted with \V:lter and the rcd Jlka!i nc sol lI -
the fi ltrale lo b~ ;!cid ificc! l'o r r~ co \' ('ry or
rion fjlrcrcd, w.lshcd with a littlc ctht:r lO rt.:-
rl'sidual ;h.:id, l'ht' pr':<.:ipit al<! ol' 6-mdho:-;y
movc unrcJ<.:ted !litro meth oxv toluene, Jnd
indo le i ~ dric'(\ in a va,' lI l1lll dt:siccator o\'.:r
aeidific:d with dii IIC I. Upo'n blow in g :lir
con ,Ilifllril' ac i(1. :lIld 1!13y hl' recrys i31l izc cl
through t ne liquid lO remo\'c dissoll'cd cth er,
l'ro m petrolcu m cther if desired,
2-ni rro 6-l1Icthox\' pllcnyl pyruvic aci d , st.: par
ate~ Ollt a ~ :l hrown oil wh icll Illar so li dif~'
slo\\'I~', Th is is collccted ane! l!ried in air.
STEP VII
STEP V
Proc"l.'d , u,ing the pro,','sSl'S for 01\IT , lIsi ng
Crude 2-nitro h-lI lctho ,\)' plll' ll y l Jlyrll\' i,' 7.5 g o r 6-llldhoxy indoJt: in pla,'e of 70 g
a-:id (23,'1) g is dis,ol\'.:d in amm onia (1-+01111 indole f or tll" li tluulll :duillinuill hydridc
o r ,RS · ;iIllIllOlll lllll hytlro, idt: Ill;Hk IIp I,) r,'dudio n , 11>,' ~2, 7 g 01' th.: IOC mClhoxy
200 mi \\,i th waler) ;md a ho l \\':,l<.:r ,olUtiOIi dcriv ati\'è , I he t'in.Ii product \V iii hl' 6-llldh-
or f~rrol!, sulfat (' (]I)() )! 01' hy ùr at"d ,Ty,;t als oxy 01\IT whidl may be II\cd in that form or

33
 co n\'erlèd lo o·hydro:>.y D ~! T (ps ilo ' yn) by Illllll0G R,\PIIY
warllling wilh a 'ol li lion o r hyd riod i..: ;lci (L ..\lIlc, i '~1!
Ch":!l!"" ! Jounu! I <) I O, .:!±.. 136
roIIO\~-=d by l'X tral' linn \Vith cther. rrolll the Oèut<dl" Ch,'lIli"hè ll Gèse ll<ch"ft Bcrichh' ! 'lO·I.P.
1020
solution mad.: b3~ i c with 31ll1ll0ni ll ill hydrox ·
Journ:d o r th e:: Amt: ri\.\ll1 (,h~m ic31 Socil.!ty 19 ] 5. 107 ,
id~. l'si lo<.:y bin is d itlicu ll (o produce and th,
ò~2
body IlllIsl cOl1 v.:rt il IO psil ocyn b~forc il is Journ:11 oi Ih e Am"ric.ln Chcm lcJI $, ' id)' 19 15. 1) 5,
a b\or bc d. ,;o il ha, no adv:mIJg.:. 297

--
- ---

34
~tlocyn .synthe$is

1I0 - C=0
I
C=O
I CII .\
CII : O

'-_______________~/~I!JOO~~ ~O)
EtOK

Dic th y l Oxal3tc
..., FòO~
N(_),________

in NII 4 0l!
0J"o
V ~ fl \
H 011

CII ] O () l'li .\
() n Il O

Co
~ I ('-('~~_'I

+
~ N
I
Il
-.::::--- - -"
( C Oe!
Ethe:
)2- -

QJ Il

('11 3
\
1\ H
/
C II
J I cther

"

35
 SUBSTITUTED TR YPTAMINES

DMT Synthesis

STEI' I 1'00111 l empaatur~ and us<'! the np p ropri:li~

ali qllo l. Sl't lIr lhl' e nt ir\! ap p;mJl llS thl: s a l ~le
Using un al'<~a of good vt'nti la t ion or a rum.: as wh \::11 add ing th;: oxalyl chl m ide. " d ci lile
hoocl. piace :1 1000 1111 fO lI ndho1toJl1 ilask in ,ll11 llh; sol l1t io l~ slo wly to Ihé IO\' wilh \ igor-
311 ice b:: lh lI si ng Ihc Sl' t-lIp in Figure' l. Ade!
400 m i co ld Jn hydrolls etiler to Ihi s Oask. in o
'.>.'hicl! 60 g indo ll' is lhen di ss () I \'~d lIsing rhL'
stirrer. To 100 mi ,lI1hyd roliS l'rhcr in 3 sCl' ara-
lOry i'u n nel ad d 50 g of oxaly l c h l orid ~ . Slowly
drip lliis sollition into lht.' vigorolls ly srirrcd
indole sollition o\'C'r a period or IO io I ~
mil1l!les. Con tinue stirring IO min ll lcs longn.
All o\\' rhe pr('cip ltatc lo scllle a f(,'w lllilllltcs
and dc'cant thc liquido Add <Inhydrolls l:r1n:r
alld Illix \Vell. A.ll o\V th is LO , <, tt k ami d<.'C:1n l
, h ~ liquill ;Iì;ain . Whl:1l salis fi~d as lo Ilw
puri ty of the pH~c i p i tali:. k avl' thl' golJtn pr\.'-
cipita te in th e. 113s1<. l'or t ll(' l1('xt slt' p whirh
illUS I rollow immcdi ah' ly. Yicid is approxi-
ma td y 100 g.

STEP Il

Di mc thylami n::- rCile ts rcadi l)' with indo le

oxalyl c hl o ridt'. U'L! a bOt:t 400 m i icc-\:old
anhyclrous n h\:[ iII I h l~ " Ime 2 neck 1000 mi Figure l
RB l1ask uscd in Step I. wilh th <, precipitate
1. J 00-500 R?\\ s?lrkkss m Oto r
in il frOlli Ste p l. Cool Ihe ice ba th fur lher
2. F.cc<.:'::tric st irrcr driver
by lE;ing sa lI an ti iCe. Es( ima k Ihe weighr 01
3. P,ddl c fl b deù st:" ing ro d
the precipi tat.:: and lIS(' 100 g indole oxaly l .~. Pul }'dh dent: st.oppcr.
chlo ri dc. For thi s wei gh l or IOC use t\'.'o 5. Wcig ~ , cd coatcù stir· b:ills
cnt ire 50 g con l:l illl:rs or dime thy lam inc ~ i nc(' 6. Dro pping fu nncl (scp,rato ry)
il wi ll noi kce p il' rhè contaj lll~ r 'l',tI is brOkl'n. 7. i 50° D~nt tu be
Cool Ih~ ~lIni ll': in con ta ine r Ill uch bL"l olV O"C S. lOOm t 2 1:~ck lUI f] "k
allel di,salve I part ami De in :; p;1rh :iDhy drolis 9. Ice ba t b-
cold d he r. Amine m :l)' be ston:d in Ih is 10. Ring ston d and d amps
solulion. For 1I~(! , wanll srock solu tio ll to

36
ou, stirring. Stir l'or ~!~ hour afte r th e additio n 0.1 N :--JaOH , ex lra ct ing thi..; solut ion in tu rn
is compleit'. all ow ing th~ tcmper3turc to risI! with ch loroform. Th(' chlo roform Iayer is
to aIllbie n t. \ 'aclIlIIll lì lter t he preci pi t ate \Isi ng dr i,cl OI'er allhydrous 1\:12 S04. ~onccntralcd.
e t her :IS :! was h. fo llowed by ~n c lh 'T-watn all ei from it D~I T cryslalli/l:s 0 11 addi lion or
\Vash. II i, b ' Iter lo slurry the e t her-wlt er pc trol eUIll e ther. Thc mo t hcr liquor can b'
wit h the prl'çipitate o d ore tiltering. Recrys- ch ronut ogr:lphed 011 a n aillmina l' o lllllln usi ng
tall izc from hot e t ha no l or frol11 3 50-50 bcnzellc-m d ha nol in a ')<) .X to O.::: ra lio.
md Il :11101- b c n l .,m o;: III i:l. I u re .

ST EP III

Prl'pa rc apparalus as in F iguro;: II. Prcp ~rc

thc indole glyoxal amid e by mclting and
castin)! illlO sti<.:k, il' c th cr is to be uSl'd 3S a
so l v<~nt. r\luminulll foil ma kes a gooel mold,
l'or casti n g picces which \Vili fil t hrough lhc
co ndcnscr. ,l\ lso a Soxhlct cx tr actor m a)' be
llscd to 3Jd thc cfI'st al s by slow solu t io n imo
the c lhcr. T Clrahyd ro tur:m, if :lVailab lc d is-
soh'c> IGA ,ln d t hc compounel j, aeldcd slowl y
in thé solut ion torm.
To 3 stirrt'd llli" l urc DI' 15 g LiAll!4 in
300 mI anhydrous <.: thcr (or TI-If ) slowly add
t he slicks (or solution) of lG ;\ unl il :10 gin
311 h<1 \'C bl'Cll a clcl~d. Ke .:p thé' rate o f rcac ti on
a l a rl'a>ollabk k"c1 o r boi l-ove r mal' O':C ur.
Stir :lIld rl'll ux l'or 90 m in ut.::s aftcr th.:: ael -
d il io ll is cOIllpk t '. Cool in :In ice-ba l il and
bcglll to c:llIt iow,ly hy d rolYlc t hl' l'om pkx
wilh d lips or ice o r a col o solulion of mctha-
noi. ,tddl'd through {hc mndcnscr .W hen there is
110 t'lIrl hl'r r,'adio n . aocl a fl'w mI cx tr3
wat <!r :111d allow to se tll e fill~l l1 y 3 nd d ccallt 5
thc l'!c;Jr Iiqu iJ into an cvapo l'ating \·esse!.
Filter (hl' rl~ sidu, ancl was h st've ral limes wilh
rt hcr-mcth:mol or TI-IF-met h:l no l. Eva po rate
thC' l'o m bllll'd extracts ano i l' n 'ccssa ry, seecl Fi!(tarc Il
thl' Ill'a vy 'ynlj1 wilh <.:r y,la ls o r DM T. Wit h l . Et her ve llt to ou tsiJe
no s,;cd Cf) q;t! s IÌlc produ ct m ay takc days o r 2. CO;1Jcn\Cr
,\ l' Il lI'ee ks lO ~rys t :t!lize. Th i, crude product 3. IOOOm l l{ B tl ask
is ackqu:lh.: t'or smoking. 111 order to purify 4 ..\lJgr.~tic stlr·blf
D:-'f1'. bcg in 3ft('r the LiA l H4 ha, bl'cn hydro- S..\bgncric stiTTcr
Iyzed with mcthal1 ol. Add 500 mI saldo 6. H,' ati~g n1 Jn t k
N:I!SO .. ..;olulion. mix ami lì ltcr. Wash w ith i . VJriae ( ('; « 7 rcphcc.j hv
ethl'r or Tllf anel neu tral ize thc filt rate with icc-bat h in bsr part)
0. 1 N IlCl . Extract with et ha in a sep;l ralOry 8. Ring stJnd Jnd ciJmps
fUllne l and nt: utr;Jli /.c the lowc r 13yel' wi t h

37
 DET

STEP l STEP 11

Same as for DMT. Refer lO notes on anhydrous ether. stirrer,

sparkless equipment. and ventilation in Ihe
STEP 11 note for t.:p I.
The color of the precipitate lighten some-
Usc 200 g d iethylamine per 100 g IOC. what a the a mine is added to the compound I.
Dicthylaminc i le s \'olatile than dimcthyl· Thc \Vater in the ether is U. cd to di olve
aminc, so cooling is not necessary. but th" aH low·molecular weight amines.
fumcs are poisonous. U e lhe same proce·
dure otherwise. Dicthyl (h:rivative is ':;Isier to STEP 111
work with.
The crystalline amide is difficult to add to
STEP nr the LiA I H4 mixturc. A Soxhlet extractor
USI: same procedure and equipment. Use may be used to add the amide by placing it
22 g indoleglyoxal dieth>'lamide. The ti nal in·belwcen the flask and condens'r. Casting
product is also casier ro purify. il inlo rods or bars is one of the impl t
method '. Tctrahydrofuran. if ava ila ble. enables
the indole glyoxal amide to be dissolved and
NOTES addcd as a solution; a procedure which i best
and fastest or ali . LiA l H4 i' a very dangerous
inl1ammable compound , especiall}' so when in
STEP I ether solution . The ether Illust be absolutely
anhydrous or a violent cffervescence occurs.
Absol u tely an hydrous etller i essentia l. destroying the LiA I f4 and crea ti ng a fi re
l\. co n lainer that has been opened previ ollsly haZ2rd. Contac t of LiA I H4-ether solution with
is no longer anhydrous. Wherc cooled re- any water, damp matcrials, or even chemica ll y
actions are necessary, remember that mois- bound \Vater sueh as cellulo e cau ·cs SpOIl-
ture i drawn to cold objcct., :lOd cold re- taneous combustion . A sarety shield made
agents, whcn Icft opcn or pourcd. bccome frOlli auto windshicld material i a musI when
quite wet. Thi applies to the initial reaction work ing with LiA I H4 in any form o Handling
in ali threc teps. A magneti c stirrer will noi LiA I H4 i' done wcaring rubbcr gloves in a
work fo r stc ps I ami Il. Thc \'igorolls wobble- dry or inert atmosphere with a millimulll of
stirrer has been found adequa te lo deliver the friction involved. Hyd rolysis of the complex
violcnt stirring nceded, especially when severa I is dangerou and hould be done slowly and
·tirring ball. are u 'ed in conjunc tion with the l'auliou Iy. U. ing an iee-bath to cool the mi x-
paddle-bar. Sparkless motors mu I be used ture.
around ether. Difficult>, in producing crystals in first
Oxal yl chioride is very tox ic alld vemila· rime should cause no conccrn since man>, or·
tio n or a fu me hood must be used. ganics need sccd crystals tO crystallize. Thc
Water va por hydrolyzes product I. pro· synlp may be used for some purposcs but be
ducing a gummy dark-rcd mass o Procced to sure to save some sccd cr)'stals if you hould
step Il as soon as pos ible. happen re gel some.

38
 REACflONS

OJ+
o O
l Il
C - l"
I I
nn
I
Il

~ ~
\ O \
,\ ~, O ~ ,

OJ 'e('~'
\\ ( ' ~
' ; ' \\ \'-
~ / \' ~ /

~
I I(H~O lromplcxJ <
]\;
Ethc r
Rd1 u x LiAIH .1 + I h- :-; I <:
I I
Il H

5ub.stLtl11td J ryptamln6s

Bib liogr~phy

Juurnal of O rgani ~ Chcmistry 23. 1977

Joulllai 01' th~ AIl1cric3Il Chèll1icJI Socicty 76,6208
JouIII31 of thc American Che l11icJI Suciety 82, 2184
Chcm. Abstr3C tS 3 , 11324

39
 ERGOT CU LTURE
AND EXTRACTION OF L YSERGIC ACID DERIVATIVES

Clnviccps p/lrpuren (F:rgot) must firs t bt!

isobted as a pure cul ture or o htaincd l'rom
I<ubber tube for
a m3inta ined collcct ion of pure cu lture st ocks.
Tll<: cu lt Ire is revitalil.t!d ami prcpar.:d l'or
innoClllat ing a large <.:ultu re by grow ing as il
small surl'a.::e culture on th e m ed iull1 describcd
below for t\Vo wct!ks a t l'H 4.
PlImp
Sucrose . . . . . . . .. 100 g.
Chick pea mC31 . . . . . 50 g.
M,kc up tù I
COl (1"° 3 )2' . . . . . . 1.0 g. litcr and .~djust
KII 2 PO+ . 0 .25 g. to pII -I with Culture Air Trap
." IenSO 4' .... .,025 g. itric acid and FI GlIKE l Jug
KCI . . . . . . . O.12"
) g. :tmmoni:l .
Au toclavc lO
FeSO 4 . 7 11 2 0 . 8. H lllg. steril ilc. mrc to I C;;. cl h anol lbing 95';t. ctlunol (ulHkr
ZnS04 . 7H 20. 3.H 1l1g. sterile conditions) . aftl~ r which. growlh is
n13intain ed un der Ih.:s' cond ili ons ior 14 (bys.
The cullure is 1113de acidic with ta r tari.: a,' id
Grcat ca1'<: lllus i be laken noi lo COll-
:tnd is homogl'niz..:d in :1 bi 'ml'r :lt maturity.
wminatc th e culture. sincc Clnviceps is a p3 ra-
After an hour. :--J1I 4011 i, ~lddl'd to adju t thr
sile :1l1d is ta kcn ov.:!r by Jny nllmber o r more
pH lo 9.U. and the solulion is t!x lradcd wilh
vigorous , Irains 01' ~ aprophyti<; fungi :llld
bcnl.t:n.: o r , h loroform-isobu la noi mix I ure.
b3c(('ri3.
Extraet with :11 'oholic IJrt aric acid solulion
Innoculat.: a numb 'r 01' largc 'urfa cc l'e l'-
3nd evaporate <juick ly in V3CU O IO d~'nl'ss.
me nts in gallon j ugs con laining the ab()\'c
R<.:<.:ovt'f the free base as needt!d by l11ak ing
mcdi3 , ll>ing the sm:tIlcr cullu n: by homo-
the lartrak basic with ammo nia to l'II 9.0 ànd
geni7ing it and using portions of it under
t!xtrac ling with chloroforl11. EV3por.l!t' lhe
,!eri I . condi tions.
<:hlorofurm in vacuu. l'rok<.:t l!te bastO from
Prior ro innocu la tion. makc an acràror (see
Iight, heal. moiswre and air.
figure I) by raJll1l1ing a largc glass tube full 01'
EXlraet io n {;ultured ergot (sce prcvious page),
cotton , fitting one h ole stoppers to the ends.
ergo r sclcroria, \i ùrni ng G lory ,,:ed,.
attaching g1ass tub in g as ,how n . a nd 3t taching
Equipmcnt : Blender
a stopper to lìl thc j ugs wit h a \'ènt tube to
Sep :Halo~' funne l
b<! ':x I<!ntlcd to a t1~sk conta ini ng a dilute sol-
Chromalography column
ulion o fhyp oc hloritc. PUI [he stoppers, tubing,
r-Ia,h c\'<lpora tor (or hair d~'(' r )
an d lìltcr in a papcr bag stapkd shut, anel
Long w:m: UV 13m p
au t oclave i!. After innocu la lion. <.:a rcfu ll y
pla<.:t! I h.: :ls:><!m bkd aera to r on the jug and Reduce Ihe makrial IO 3 finc powder in a
force ai r Ihrough il in lo tht! sol ul ion . bkndcr. II' moisl or wet, dry firs!. prefer3bly
~hintain aeration at 25~ in the absc nc<.: of in \' acuo. P3ck thc powdt!r in a brg.: chrol11a-
bright lighl s. Afl<!r tcn days, adj l1 s1 thc cui- tography coll1m n as a slurry with ligroinc or

41
 lighter fl uid . S03 k ol"ernight a ll d drip (pm:o- tion \Vith an aci d- ba sl' indicator and cst inu tc
l at~) slow ly uilt ii the 'olvellt is g r<!3sç-fn:~e . tht! number 01' m oles 0 1' alkaloid pr<:scn t by
This tJk cs abou t 5 ml!gm. of sèeds . bu t Ic~;s tit ratin g with tbis acido ~I os t of tb e r('sidlle
on ergot. When t he fa ts are thu s rem oved . sbou ld be di sso lved or susp.:ndecl . Transft'r
an am m o n i ac~ 1 chloro fo rtn sol u tion is wa,bed th e so lu tiol1 to 3 sepa ratory funne l. wasbing
slow ly throllgh. Pre.parc thi so llltion by shak- th e cV;lpo r;lting ve:scl with cxt r:.l :.lei d . lI-bk~
ing 100 mi con NH4011 in 900 mi chloro- basi.: w ith t\aHCO.< solu tion. "dd 'q u;1 1 \'01-
fonn. 'Ilte hOtlOIll chloroform layt!r is drawll UIllC 01' CHCl 3_ Shakt! thoroughly, !t' t ,tand
off wit h th e help 0 1';1 separa tory funnd. Th i, and n:movl.: the bottom lay~r. Ext ra,·t ag,lin
chlorotorm wash : h oul Li bl' dri ppcd slowly with chl oro form. R,'dlle~ th~ combi Jl <!d chloro-
through as SOOIl :b tile li groi nc t'rae ti on shows ìo rm extrJc t, IO a soli cl as before. Se raJ1c l hl'
no gr~asl.: fil m wh en evapo rat eli in a wa teh so licl IIp wit b a staiJlIe~s ~ t ec l o;p:l tub. T his
glas.',. Collect anu S<lVe th e ch loroform cxtract powcler can be u"ed dir~etly IO lll;Jk~ th ~
ul1 til it uoes n ' t nllor~sc~ o n l'vaporation or a hydrazid.: . ASè o rb ic acid is IISlIally u".:c1 as ,l
drop 0 11 il wat ch gJJss. Evaporat e thi, solu- J1 r~ ,er\'ing agelll.
tion lIs ing a hair dri cr o r cv~n be ttero a fbsh SmUOGRAPHY
evaporator. W;l,h t he rl'siclu(' with J y;r. tar- Chcnu.;al :\bstro.:ts q. 1 30~ I
tari e :l,id solu tiol1. Colo r thl:' 3 ~. tar taric ,,, ILI- Chern i,'"1 .'\ bst rJc(s tiQ . 1134'i

42
 SYNTHESIS OF LS D-25

Preparator)' arr;ingcmcn ts PR EPARATION :t I

Suning material may be any Iyscrgie acid Step I - VSC' YclIo\\' Ligh t
derivative, from Ckl.'ic.:eps purpurL'c1 (c!rgot) 011 Piace ol1e \'olume of powdcrcd ergot alk,l-
ryc grJin or from culture, from lpoll/e<? (morn- loiel material in a tiny rounelbottom f1ask anel
ing glo~y) sccds. or t'rom s~'l1{hecic sourees. :lud twu VO IUIllI!S 01' 3nhyd rous hyelr:lz in e.
Prepl rat ioll #1 uses an)' amide. or Iysergic An alternale pro\:etlure l"e~ a sca led tube in
aeid a~ st~rring matcri~1. Preparations #2 and
=" Illll,t start with Iysergic acid onl}'. pre-
p~rc I t'rom th c amidcs as follo\\'s:
which the rcag ' lltS :lre: hcat..:eI at I I 2"c, Thc
miXlllre i ~ rdlllxcd (or heatecl) l'or 30 minutes.
Wilh ;1l1 opm cond\:lls ~r. kl'l'p <.In in..:r l atlllos-
IO g 01' ,1I1y Iysergic a 'id ami(k t'rom v3riolls p!ler..: 011 the' reac tion . Add I .: volum cs H~O
natural soun:cs is dissolved in 200 mi of l11t!th- anel boil 15 minutes. On eooling in the r.:-
anoh' KOH solutiol1 nl1d the 11\l:thal1 ol rl'- frigerator. i soly~ergic a<.: icl hydruide is crl's-
mov~d illlll1 'diate l)' in \·.lCUO. The residut! is
ta l! ized .
trc3t\:d with 200 mi 01 an 8'} :l( l lIC()lI~ solll-
tio l1 of KOH and the mixtllrc hC:ltcd 011 J SI"p II - Usc Red Liglll
~t.:alll !l:llh l'or (>Il\: hO llr. :\ strcam of t\~ gas CllJlI ali r,'O!!l'llts :1I1d havc ie~ ha ndy . Dis-
is passo:d throtlg,h the' fbsk duri ng hcatillg and solve ~.82 g 0 1 the hydraL itl\: r3pidly in 100
the ~\' ol\'eel :-J II _: in lhe g:h ,trt'am 1113y bc 1111 0.1 1\ ice-c ulti Ilei ll>lllg 3n ice b:lth lo
litr:!kd i:l I ICl to fo lloll' the rC:l\:t ion. 'fh" k,"" t he reactio ll \'t:<sel ;J( O' . 100111 1 iC\:-\,' old
:t!kal ine' ,0lutiol1 is l11adc n':lItral lo l'Ollgo le J 0.1 1\ :-:31\0 ~ is ad d.:u anel aftcr 2 to 3 min -
with tart,lric a\:id. fil t ~r~d. ekanC'd hy l'Xtract- utes l'i)!ul'OUS st irrin g. 130 mi morI! !ICI is ~d ­
ing Il il h <:Iher. th~ :lq\le\lU~ ,01\lt101l filt erc d de' d dropwis<! \Vit h vigu roll'; slirring agail1 111 311
:lIld ~ \':11 o rakd . Di!!(',t I~ith 1>-lt'OI-1 to remOI',' ice b:1!h. After 5 minutes. ncu lraliu t Il<' solu·
,omc of the colon:d m.llcrial from th ~ crys tal (ion witll ;\31-1C03 'alur;l!cd sol. ond extrad
of Iyscrgic acido with crher. RC l11 0vc chc ~(lUC()lIS ,ulution and
/\lr:1n1.'': th,' lighling in l!t\: !a ll oralOry ,imi- rry tu dissolv c the gtImmy ~ubstancc in ether.
brl)' (O tll:!( ot a da rk room. U-l' p!tO IO- :\ djust thc cthcr sulutiun b~' adding 3 g d icth)'l-
gr:Jphie red anel yel!ow saret)' light> si nl" ami nc per 300 mI ethcr eXTrlCt. Allo\\' to
lyse'I').!iè ar id de' r i \·~ t i \' c,; are <le,:olllposcd by ~land in dark , gradually warming up to 20·
lighl. ,\ weak. lung W3V': u l tr~viokt souree is over a pcriod uf 24 hours. Evaporate in
con\'eniL:nl l} Ill:!d l'ro m th~ purpk gla~~ lìlt"r VleUlll11 ~lI1d treat as indicated in thc puri-
u~'d in th" 19:0 Ford da,h ligillinf; Syst"Ill. fiC:ltion . <:ction for con\'ersion of iso-Iyscrgic
A small tUI1g..;;tt'11 bll lh will pro\'ide ~ nou gh amidc:s tu lyscrgic ;lcid :un ides.
ligI! t. PR EPAR ATI ON :;2
Il ;l\e p k n(~ ()f alullli nulll l'oil hamly to
(O\" 'r re'J~"nts ~nJ prodUC I'; w!t<:n light is Str p I - Usc Yellow Ligh t
pres..:nt. Ru bber glov~, IllL"t lJe l'10m J ue to 5.-'6 g 01' d-Iy-;ergi c ae'i d are suspcnded in
thc' h ig.hly puiso!luUS nature of t!rgol alka loids. l ~5 mi o r a-.:ctol1i tril<: and thc sll'p~nsion
1\ ha ir dryc r. or. mu ch be(ter. a f1 3sh evapora- coolt:d IO abOtll -20°(' in a ba th or ~':'lO n~
tor. I lle' Cesso ry CO spced up stC ps whc!'c C'vap- coolee! with dry iCI'. To lhc su,prlblon b
or:!tion is n cc\!ss~n· . auded 3 cold (-~O') solution 01' 8.82 g o f tri -

43
 lllloroJc<:tic anhydrid ~ in ì 5 m I 01' ;JcC' [Oni- I I li ters 01' d im ,t hylfofm <lmide (fr~s h ly cl is-
t rilé'. T he m i" tu n: is 3 11 ow~ eI tO stand :t t _20 0 ti lkd lIn d er n:d ucL' d pre~"urc). The comkm.:r
for a bo ll l I Vi homs during whi .:!l limo.! lh ,~ an cl cl roPPlllg funnd arI.' bO l h p rolecled ag:1i n, t
'\Ispc nckel ma l e ria l clisso lv cs. anel lh,' d-I yse r- almosph.: riè mois t mc. 2 Ib of sulfu r lri o"idc
gic: acid i, co nver ted lO I ho:: Jll i,, ~d anhydnd~ (SlIlfa n B ) are illtroduc.: d t!ropw ise, vèry
of Iysc rgic i1lllll riI1 uo ro acTl ic aci d s. T h c m i"cd calltiollsly \V it h s t irrint!. during 4 l o 5 hou rs.
anhyel ridc ,a n be $<,para t C'd in Ihe fo r m of an T hc tem pe rat ure is k,'p l a t O_5 0 t h rougholl t
oil by c\'aporaling th e so lvcnt III \"acuo al a lhe :\cl c! ilion. After Ihe :\dd it ion is coll1p lde,
lemI' ' ral ll n: b ' Io w abollt 0 °. bUI Ihis is nOI Ihc mixtllr.: i~ slirr.:t! ror l - ~ hours until SO Ill I.'
Il~c<:s~dry . Evc ry lhing musi be k<,p l anhy- s.: para t.:d. -:ryslallin.: slI lfm t rio"icl.:-dil1l<'thy l,
drous . forlll,lI11idc ,,:ol11pkx has dissolved . T h c reagent
i, t ra!lsrnred IO 311 air-l ight J lI tolllati' pipètl~
Sle p Il Usc R ccl Ligh l
for cOII\'\!nil.'n t displ!lI-ing, a nd kepl in Il,,:
Th~ 'Ol lll ioll of m ixc d a n hyclrid', in ac:<:- c·old. A llhough thl' rl'3i!,'I1l. w hil'll is colorle>s.
lonitrik t'rom S lq) I is ad d cd lO I SO m I of ;J may chang.: IO ycllow :\ncl rcd, 11< .: flìcicncy
se,onel ,o lut ioll of a.:c to nit ri k L'ontallllng 7. 6 relllains 1I11illlluired for I hr,,: IO four mo nt ll s
g of dic thybm ilw. T he mix tun: is hc ld in t lh' in co ld ';lOrag\.' . An a li quo t is d issol \" 'd in
d,H: :It rOOITl tcmpe ralUre for aho ll l 2 hO ll rs . wate r alICI litrated \Vit h -;t;lI1e1 ard NaO H IO a
T h<, 3l'd oni t ril,' is c\'apor:\ l ed in vacuo , Jc:l\'ing ph enolphtll:d l.'in I.'lId poillt.
J r,'sic!lI c of I.S D , ~5 plu< oth~r il1lpur iti('s . Th c

r 's iduc is d is,o lved in 150 mI or chloroform SlC'p II I - Usc I{ cd Li ~h l

:lIld ~ O ili I of ice \l'a l er. The .:h loroform lay,'r A solullon uf 7. 1.- g 01' d- Iy sl.'rgi c acid
is n:mO"é't! ancl Ih, a'1l1 <,oll., lay.:r is eXIr:\c\l!d 1110no h yt!r:J I,' (:!5 IllIllOI) a lld 1.0(\ g 01' lilhi,
w lth sC\'t' r;d porlions 01' c h loroform. Th e lllll hyt!roxit!~ hyJr31" (25 11111101) in 200mlof
chloroform >,o rt iOlb a rt: combincd anel in "kOH is prqxl ret! . r h' soh'\!111 is dist il kd on
lur n . "';I<hed wilh four 50 1111 Jlortion ~ (lf l he '>l.:am b:ll h und e r r~dllc~d p[(:·"lIre. T h.:
i,',',w ld wal,'r Th e ch loro fo r l11 SOllltioll i< Ihen rcsidu or ~b"-lik,, li lh illll1 Iysngat~ is (IIs-
dried o \'<,r 3n Ìl yd rous :-';'\ 2S0'1 ,11It! ':\'3 por 3Ie d 'olv'd in ,WO m I u r :\IlhyJrous dilllet h yl rorm-
in \ a(lto. am id e:. From Ihi ;. SOlutlO Il about ~OO 1111 of
th~ d illlcl hyl formami d ,' i, disli lkd off ;1 1
15 111 111 pressutl: through J I 2-i nch h~lic ' ~
PR EPARA TlON id
packed l'n lum J1 . Th,' r<!slIlting :1I1hy<l roll< sClIll -
T h t: fo ll owil1g procèdm~ gi \'c$ good yielcl tion ui" lith illlll I ysl!Tgal~ kt'1 b~h i nt! i~ coo k d
:lIld " \'~ r y fasI wilh h ul<' "o-Iys.:rg i.: :1cid IO O· :111<1, \',It h , t irr ing. (f;.';lted rap idly Wi l h
bl'illg product.:d. how.:\'t'r, th e slo icllorlletr) 500 mI of SO ,- (),,!F solllti(ln lI - O~ lIloia r ).
Ill USt b... ex:\<.:t Or y i (;It!~ \Vili d rop . Th' mix lurl' is slirr~d in t he co ld for I O
SI ':: p I - Use \\'hi l e Li gia minutes a!l d l hen 9.14 g II ~5.0 mmo l) of
Sul fur trioxidl! i, p roduceel in a n :1!1hydrolls eli\.'thy I3min<.' is addl.'d. l'h .' sti rring and wo!i ng
staI': by c3 r.:flllly d~..:()mpos i ng :Illhyd rous 1'<'[ , are ;.:ont inued l'o r IO m inutes longn, whcn
TIC su lfal' al apprOxi1ll3t .:l y 480°C. Stor" un - 400 mI of w:ltn i, ad d ,'d to de,'ol1\po,~ l h.:
de l' ;lI1 hydrous cond ilions. rl'3ct ion co mp I '\. Art 'r m ixlIlg Ihoro ll gh ly,
200 m I of s3tural 'd :1l)lIl'OUS s3l ine' solution is
Step Il - Vse White Li ght a dded , Th ' amide prodUcI i~ isob lcd by rc-
A clrdully dricd 22 liter l{l~ tlas k fit Icd pcat<?d 'x t r;tcliOIl "'llh 500 mI portiolls of
with :111 ièl.' bath, condl! nser, t! ropp in g fun n,'1 I.'t h ykn,' dic'lllor iele . Th" ~ol11bincd l!X I r; I~1 is
and Illcch:lIl ica l stirrer is chargl.'eI wilh IO IO Jrie d and t hen conce nlral.:d to a ,y rup li nd a

44
r,:òlI<:ed preSSllr~, Do noI h~al thl' syrup p:tratiollS #1 or :: ~ , E\'.lporate iII vac' uo :md
duri llg conccntration, Thl.' LSD lIla}' crystal- duollla lograph a, i Il t hl' l'n:\" ious stt'p,
lilC ou\. but [hc .:ryslals allò the m()lh~r Salvage
liquor may be ,hromalographed Jecord ill); [O :-Jeulr;llizl' alI Idl ov,'r solutions and resi-
the instrudion'i 011 pur ifil:ation, dues \l'ilh 1'\aIlCO,; ;lIId evaporate in \':Ie'UO
PUR IFICAT IO:\ OF LSD-25 lO low \'Ohlllll', rxlr;k' t \\'ilh JIllIllO!lial'al
'l'hl' materi;t! ohtained by Jny 01' tlll:sc three dlloroform alld ,'vaporalc Ih:: .:xtrJ" to òry-
pr~'paraliolls may contain both Iysl'r~i<: acid Iless, Thi, residue ma} be run through I he
alld iSl}-lys.:f)!i-: a,id amides, Prl'p;tration :: I \\'hok pro, ... ss again :md lIlore I.SD \\'111 h,'
con lai ll s mos t Iy iso- lysl.'rgil' tli,'thylamid,' and producnl.
musI be convl'rll'd prior lO Sl'lXlralion, l'or Sloragr 31ld USl'
Ihis m;lleri al, go to SI.:p Il firs\. Ly~.rgi, al'id c'ompollllds (am on)! t!l,'m
Slep I - Use IJarkroom antl Follo\\' With LSD) 3r. l:Ilslabk to 11I:al, light Jnò O,\ ygl' n,
I.ong \bvc UV In any t'onn it help" lo ;tdtl a,,:orhic acid a.,
an anli·oxidanl. kl,,'ping 111\' l'ontJinl'f tighlly
l'hl' material is dissolwd in a Ihn:l' ttl 011"
mixturl' 01' hl'lIl.l'lll: in chloToform, Pack a dosl'd, li~hl-lighl \\'ith aluminlllll fo il. ,lIld III
<.:hromalography <.:olullln with a ,Iurr)' 01' b;l~ic'
a rdriger:ltor.
alumin,1 in b,'nz,'Il(' so rhat a onl'-indl ('olumll l'ad: aging t'or Il s,' prt'senh m,my po~sibili·
IÌI.'s, partially dII,' lo t 11(' incT..:dit-- ly ,m,IlI
is ,ix in dIe, long, Dr'lin the solwnl lo Ihe 101'
01' Ihe ;llum illa coIllllln and l'arl'fully aòò ali dosagc' in\'oln'd , hl'~1 a bio-a,;,;a} ot Ih ,' 1'1111 '
;t1iquol 01' thl' I. SD·solvent Sollilion .:onl:tin· t'il'd so lllt ion IS m,t<k, then il m;w be lIIea '
ing SO mi of so lvrnt ami I g I.SD , RUIl this surcJ by tlH: volullle of thc soh-ent it is in, I h,'
soluti')11 through Ihc COIUlllll, followillg the: sol\'enl Illa}' be "\':tporal<:d onlo a w,'igh ,'d,
fask'il Illo\'ing blu.: Iluor,'sèl'nl b:md, Ancr it ,'akubll'ò alllounl of som.: Inac' ti",' l'(1wòc'r
ha, b<:l'n coll<','t",!. strip the rl'maining l1lalaial sudI as dl:tlk, ,ug.lr or baking ,od,1. '1111,
from the c'olullln by wa,hing with MI'OII. U,l' bulk} powdn m.l}" h,' ";bily "I1.'al" l, I.II<'d iII
Ihe UV lighl 'l'aringly òuring thi" pro..: ... durl.' w,'ighabk porlion,. It IS :td\'antagcù ll ' lo ,Idd
.J tr.l..:e or òry asc'orbi ..' :tl'IÒ to th .., dried l' O \\"
to prl'\"l'm ,'xcl'ssin: damag(' to lhl' l'ompounds,
1:\':lpor:lt" th,' se,ond fr:H: lion in V;t,UO ;lIld dcr~, SlIgar l'ub,'s oft'n ;1 h,md~' but cx trclllt'ly

sct asilk l'or Stc'P Il. Th,' fr.lc:tion , onl:lining notorious m<:thod of ,b,pl'nsing, Otlwl mdh·
tlll' purl' LSD is éonÙ'ntr:ltl'Ò in vanto ami ods ;m' without II\lmbcr, hl'!'\,' bc'in!! orfeor,'d
Ihc syl'llp willc'rystallizl' ~lo\\'ly, This materia I ju;;t a ti:\\' ol'<.:a~Ìllnally Il,,,,d by th,' nilllin,t!
may hl.' convertt:d to th ... lartrat,' by tartarii: l'lèmcnt. G<.:lalin ~apsuks art' t:o:tled \\'1111
aeiò and Ilw LSD lartralc ,:ollvenien tly crp' thl.' liquid SOilllioll ,md Ihe çap~uks til"'d
t,llil.ed, MP I 90-196 ~ with an inert sllbsl:tn..:e , Dcco}', slleh JS th"
inert mixturl' mighl in<:lud,' a trae.: 01' bro\\'11
Step Il - Use Re.! Light color. a traCl! of qllinine t'or tlllorCSCl'nn', :lIld
Di",ol",: th,' r.:sidue d~ri\·l'd t'rom Ihe llleth- a I rac.: OfsOIll C rdil I ivdy nUIl-!o\ ic ,0111 puu ni!
;11101 ~lnPl'ing 01' Ihl.' .:olullln in a lIlinirnUlll \~hich n,'arl)' mimks Ih ... inira -rl'd ,p ~ drll:n
arnolllll of :,kohol. Adel !\Vicl' thal \'OIIlIlH: or of LSD , ror tran~port, :t ~l1luR~lcr Illight
4 :\ <tkoholi, KOH Solulion and allow li1l: .1<11'01';110: a ,on,ider:!bk ;lIl!Ollnt onl~) a p<h'k-
lIliXIlIrc' lo sla nò at roOlll tl'mpl'fa IUr,' l'or l't h:lI1dkcrchic'f or onlo a Sht' d o r paprr, pro-
s':\'l'ral hOllr~, N.u tralil. t.! wilh dilllk HCI, 1Il;,ke viding lhe ~olllti()n \\':lS prop"tly decol<,rilnl
sligh ll y hasi-: wilh 1'111 4 011 ami ,xtrad \l'ith hefor,' slldl I r,'a I nll'1l t. TheSè' ulldcrh,lI l<kd
l'!llorot'll rm o r cthykll~ d ich loride as in p rc~- l1l èthods are u'l'd by .:riminal, to ;tvoiJ l'un i·

45
 tive action by law en forcement enthusiasts. BIBLIOGRAPHY
One gram of pure LSD , if used in a truly Chemical Abstracts ~ 10740
enlightcned carcful manncr can be me door Chelllical Abstracts ~ 1499 c
to a magnificenl ex pericncc to ne arly 3,000 Chemical Abstracts :U, 2450 d
Journal o r Organic Chcmistry .~ 368 & 370
individua ls. Used furlively an d in ignorance, Journal o r Biolo!(ical Chcmistry .lQi, 547
the same amollnt may bring lerrible confus- Paten t ap plication serial #473 . 443 by Eli Lilly
ion and abjec l terror to nearly one thollsand Co .. December 6. 1954.
of Ihese.

46
 STP

In thc future man)' more hallucinogcnic Any attempt to order this compound will bring
drugs will be devcloped, some of which will the purchaser IO the anention of agents of
be safer and more pleasant than any avail- the Just ice Dcpartmcnt. To synthcsizc this
able now; othc:rs treacherously poisonous or compound involves lengthy and expensive pro-
othef\vise unreliablc as the drug known as cedures and a suitable synthesis is nor avail-
STP often is. ablc IO the editors. Man)' other methoxy am-
STP, thc Dow Chemieal Company drug phctamines are active hallucinogens similar
known to them as DOM, is :ln amphetami ne IO STP, but most have che disadvantage of
closely related IO benzedrine. The correct having too long an effect, which can be quitc
name is 2, 5 dimcthox)' 4 meth)'l ampheta- unpleasant if one has a bad trip.
mine or 1,(2, 5 dimethoxy 4 mcth)'l) phenyl
B ibliogr3phy
2 amino propane. This drug is synthesized in
"Chcmical and Engineering News" VoI. 46, No. 12
the same manner as benzedrine, provided the pp. 32-38.
difficult tO obtain intcrmediate, 2, 5 dimeth- Fiescr and Ficscr. Organi c Chcmisuy, 3rd Editioo,
oxy 4 methyl phcnyl acetone, is avail:lblc. p.501

5JP

47
 Procuremcnt of Necessary Items and Illicit ex tractions, such as mcscaline from
Prohibitions Thcreon Peyotc, are dcteeted when watchflll agents
not ice amateurs buying a sequence of simple
The appar:ltus ne cessar)' fo r these opera- chemicals :md solvents. To an)' tra incd per-
tions can casily be obtained from scientific son such an assortmelH of materials is plainly
supply houses or in some instances, can be saying, " I am cxtraeting mcscaline." The out-
madc at home. The laboratory where the work law chcmist thcreforc is quitc cautiou s in pur-
is to be done must not bc in thc V.S. unlcss chasing certain groups of materials l'rom single
it is with specia l FDA or Rureau of Narcotics eompanies or from several companies at one
:md Dang<:rous Drugs approvai. Crilllinais and time.
fugi t ives from the I:lw use either a legitilllatc A n}' Icgitimate chemist mUH not ancmpt
commerciai or educational laboratory; or con- lO pllrchase ali)' 01' the following in the U.S.,
struct a home lab with adeguate water, \'enti- unless he has a solid and Icgiti matc use for
I:Hion, a fire extinguisher and light enough them.
sccurity so ncither fr iends nor neighbors are
aware of its existance. Rcstrielcd or walehcd rcagcncs
Mcn:ly the altempt to purchase one of (dcsecnding order oi illlpOrt3nce)
cerrain chemicals necessarI' in several of the Lyscrgic ~çi d
pwrcdures \ViII bri ng an irnrnedi~tc investiga- Ergolamine (alld o.h cr ergol alkaloids)
ti on 01' the buyer by the Bureau of l\ arcot ics Ol i"erol
Citral
and I},lngerou~ Drugs. Failu re to provide a 3, ·1 , 5 Trimerhox)' ocozaldchydc
goo.! (and wc do mcan legai) use fo r an)' and Lithium aluminum h)'dridc
ali of tht:st: cht:micals wi ll me:m th:n the vic- Boron tritluoridc
rilll not onl)' docs Ilot get thc rcagcms, but 3, 4, 5 Trimcthox)' henloic a,id
will be w:ltched by the BlITe:lu 's secret agents Ox.lyl ehloridc
Diclhylaminc
for several years. Legitimatc labs are liabk to
Dimcthylaminc
inspcc tion and ma}' be rcqllired to keep an Suliur lrioxidc (Sull'lo B)
accollnting of restricted chelllicais. Law-ab iding Trillu o't"o:\cè t i..: acid
organizations are appalled hy the chcmi~t who H)'dralinc (aohydr<>us)
obtains rcagcnts l'rom his friend ly underground Indole
Pukgo llc
supplit:r or f rom a fri enJ who works for a
3, 5 Dinilrobcnl.<l)'1 chloride
brge laborator)' or supply house. Ikw:lre of 2, 6 Dinitrò luluenè
the small laboratory suppl)' company; the)'
are ofren a poliee fron t although they catch
more inllocent lab operators t han drug pushers. Il illUSI be dcarly poi nted out tha t many
IIkgal drug makcrs use longcr, more in- things throughout this lll:lIlual have reccnt l)'
volvcd synrhetÌ\: mcrhods ueeause th e eom- becoIllc unlawful ;md no one should C\'er
mor.er stJning rcagcnts make dctect ion by break the Ia w. Therefore, anyon e arrcmpring
thc Bureau more difficult. Thcsc samc methods to pursue the eO\lTse outlined herein (in
are induded for the Icgi ti matè chemist onl)' cOll ntr ies where prohibi teJ) IIIU~t be willing to
hCC:lllst' thc starri ng materi:lls are kss cxpen- shollider the bllrden 01' per~eclltion which may
si\'C ami commonly obtainablr. Kee p in mind, f:dl upon hirn. Since the rcligious user ami
howcver, anyone purch:lsing a numbcr of chemist are unfortunarcly not immune to legai
rhemicals (cspecially organi es) who is nor con- fl~tr i blltion, the cdiwrs sincerdy hope that
nected wirh :l Icgitimatc lah will likcly draw no one wi ll be forced to Illanyr himscl f
Sllsplclon. through his incorre::ct use of this guidc-book.

48
 HOMEBUI LT LABORATORY EQUlPMENT

Lab equipmenr is one of thc major costs c1cmenrs to heavier terminals for easy con-
in sctti ng up a good home lab. With ;l little nection to a voltagc controller. Dry the mantle
ingenuity. most neeessary equipment and a in air or in an oven before connect ing any
few insrruments may be built with littlc cost e1ectricity, as electrolysis will dissoh'c thc
and only a moderate amount of time and e1ement.
effort. One must judge for oneself if certain Magnetie Stirrer
equipment may be built or if it must be pur- Get a small induction motor as is used in
chased. Where glassware is ncedcd, for instance,
small fans and tapc-recorders. Use a horseshoc
it is often most economical in the long-run to
magnet with a ho le in the curve or makc a
buy apparatus with ground glass joints since
c1amp base. Do not try to machine alni co.
many reactions need all-glass equipment and
Securc and linc-up the magnet on the motor
tight joints to contai n corrosive and danger-
shaft (sce Figure 2) and mount the motor
ous chemicals.
in a suitablc framcwork. An asbestos sh ing1e
M :II1)' pieces of equipmem are overp riced
works as a heat-proof cover and will not drag
due to small demand or willingncss to spend ex-
on the magnct as a metal wi ll do. Fashion the
cess grant moneys to equally willing suppliers
stirbar by sealing a small ba r magnet in glass
on other equipment. On the following pages
or pol}'ethylene or bu}' a teflon stir bar. The
are instructions and d iagrams giving most of
specd is controlled with the use of a variac
thc information necessary to the building of voltage n:gu lator.
several different picces of laboratory appara-
tus. For furrhcr ideas, consult thc "Amateur Balance
Scientist" section in the Scientific AmeriC:1I1 The bai ance ma}' be built almost entirely
magaz ine. out of wood, heavy wire, glass tubing (split
Heuting Mantles Icngrhwise) and singlt.~edge stainless ejector-
Heating mantles cost abour 530-$40 from type razor blades.
scientifie houses but can be madc at home to Thc criticaI faetors in setting up a balancc
fit any use for about SI each. are:
Use asbestos insulating cement availablc l. Distancc bctwecn side-arm knife edges to
from a heating contraetor's supply house or the centraI knife edge must be exactly
make }' our own from a mixture of I Ib. port- thc same.
Iand cemcnt to 1 Ib. asbestos fiber . Prcpare 2. The center of gral'ity must be slighrl>'
thc flask or bcaker to be used as a form by below the centraI knifc c:dge fulcrum .
painting a layer of hor paraffin on thc surface 3. Sensitivity is adjusted to optimum by
tu be covcrcd. (see Figure I) Mount thc model
weighting thc indicator needle and by
upside·down and begin by pressing the bcnd ing the arms.
doughy-wet cement in a layer. Arrangc coi I Scc Figure 3 for the approximate larout and
nichrome hcating c1emenr in the desired pac- construction.
tcrn and eover with more cemento Rcad dir- Common wcighrs:
ections on elcmenr spool for measuring cnough dirne - 2.5 grams
wire lO givc thc desired watt age. Mold a good nickle - 5.0 gms
layer of the insulating cement over the element quarter - 6. 125 gms
to gi\'c good insulation. Anchor the ends of th c half - 12.25 gn1S.

49
 Wobblc Stirrer Drying Oven and Evaporator
Vse an induction motor (brush motors cause Vse a kitchen stovc oven, rurning the set-
sparks) and rig a pullcy system to dccrease the ting to 200 0 F and propping the door 2" open
specd te 2()().400 rpm. A ttach an ccccntric- ro prcvc:nt overhcating. For int1;lmm a blc~. use
plate to the drive shafr and makc a long stirrer only an e1cctric oven, preferably ()nc withollt
by putting a steel welding rod in a polyethy- glowing c1cmcnts. For rc:moving large \"olllmcs
lene 'A inch tube, making a flat padd1c at the of volatile solvent, lise an old hair dl)'cr in a
bottom (see Figure 4). Thc stop per must havc wcll-vemilatcd arca.
an hour glass shaped hole or flexible diaphram
which will allow the rod to wobble, but not
necessarily turno Always remember thar SOllle
hot solvcnts (chloroform or bcm:ene) cause
polyerhylene to crack or dissolve and su bsti-
tures may have to be found in cenain cases.
(Teflon)
Wcighted polyethylcne balls or small mar-
bk~ ma)' be used as stirring aids.

Supports
Ring stands and rings ma)' he madc out of
s[ccl plate and rodo ($Ce Figure 5)

Vacuum Pump
Aver)' go od and inexpensivc vacuum pump
may he made from rhe eompressor of an old
refrigerator or freezer. Certain refrigerator
compressors have three 1cads. The center lead
is the starting winding and is nc:eessary only
to overcome the inertia of rhc: compressor
during rhe first two or three seconds of opera-
tion. Connect the leads to two switches using
a single polc-singlc throw switch and a momcn-
tar)' SPST switch (see figure 6). Operate both
switches togethcr, rclc asing the momentary
switch as soon as the compressor motor stans.
li. colcl trap (see Figure 6) made \\~th a ther-
mos bortle full of dry ice and a solvenr such
as acetone or gasoline through which a V-rubc
passes will help prorect the pump from thc
corrosive gasscs cncounrered in many vacuum
distillations. A primal)' trap of ice water will
hc:lp keep the colder trap from plugging quitc
as fasr as it is sometimes prone to do.

50
 FIGURE)

Asbcstos ccmcnt body

can for support

Wire ~I~ment patt~rns

PIGURE 2

magnstiC stirrer-
Shect Asbcstos
B1r Magnct
IN si
Glass or plastic
()} rube O
Finishcd Stirbar

51
 FIGURE 3

Centcr
r:Izor cdgc
.nd bea r in~
(splir gla~ tube)
si de arm hearing
(split gla." rube)

arm liitér

pointcr ~dj uster \\ eight

Pa n
Pan dampe r

l! if:'-\1- J=~-=..::.-:...--==.::=====--:.rISt..:::-==
==== =~~l
:
'.,' ::'::. -:....--====
rll::: . "7' fl alance 3rm Lifter coorrol .. J

Pan
,bmpcr
ùlntro!

52
 Reduction
FIGUKE 4

U
,haft lO
ce'centric
cli~"

Srirrcr .\\cchanism

Snr Bali

• L.ead pellet
polrcthdcnc stoppcr

Pel let ,oatcd

wah polycthrlcnc

53
 F IGURE 5 FIGURE 6

supports VacUlltn
pump

Ex holll SI

l/," Roe! bent Cold

t
and weld{"e!

'h o, Roe!

Ring
Stancl

dry i~e ano

A~c {Onè

11 0 V
'à" Pi ace
t' C

54
 Thc use of psychedelie drugs in an anempt p. 9 - glyph from Montc Alban, stella 9; god
to seek personally relevane symbols is as descends from thc sky.
ancient as ehe compulsion to symbolizc. The
illustrations in this book are intcnded tO in- p. l O - Al/ab is tbe Past a11d tbe Future -
dicate the stru ctural similarities of symbols Moslem talismano
from man}' culturcs and periods, derived from
both drug and non·drug inspircd sourees. p. Il - from stone camposanto or gravemarker,
Diverse rcligious and mcditional approaehes Tecolote. Mexico.
te the centraI themes of ercation, death,
:md rc:cyclation wit hin a universal conseious- p. 26 - the Sbou - Chinese symbol bascd on
ness ind icate a prcoccupaeion with personal the spiraI, meaning happiness.
awarencss and harmony whieh is also the
prcsent impetus for the \lse of psyehedelie p. 29 - carvcd mushroom stone - Formative
drugs. (Miraflores, Kami nal juyu) Guatamala.

p. 31 - triple spi raI - from Syrian cylinder seal,

18-17th C. B.C. Thc spirai is a multicultural
mo tif representing eternaI motion. The closed
ha lf-titlc page - Chincse talisman against evil spiraI, as in the infinity symbol, is cspecially
influences. Thc yin-yang is surrounded by t he powcrful. Three was aver)' im portant numbcr
eight trigrams; the sequence dcterm ines the in carly Mesopotamia, meaning genera tive
intene. union - ma le, female , child.

tide pagc - the Lonls and the egg - p. 34 - l3uddhist Whecl of the Law (Darmacha-
Thc Hindu /13uddhist representation of the kra) Sanchi , India. This is a common image in
relationship between the Cosmie egg and the )udaism & Christianity also - the axlc ttee
Buddha ; between visual-outer and inner knowl- ascends from earth to sun, through the su n
edge. This rcscmblc:s in form the Assyrian ttcc door , into the world beyond.
on pagc: 50 and the l3uddhist wheel on page
34. Thc path leads rhrough receptivity to p.42 - the all-sceing cye, common ro ali major
un it)'. a concert also of the Christia n chali ce. rel igions as a symbol of om nipotcn ce.

p. I "Om mani padhma hum" p. 46 - the god of Light, Ahuramazda

Ach semenian cylindcr seal abour 500 B.C.
p. 3 Buddist "parm" in form of Lotus sced
p. 50 - trce-of-life from an Assyrian bas relid.
p. 4 Charlestewn graveston e -
prerevolution colonial

p. 6 - Medieval sign fo r " thc inrcllcet in action."

baek pagc - female mandrake - Medieval
p. 7 - Sbab Abbas - Persian ornament, found woodcu t representing the mandrake plant
in 17th century rug, represcnting the lily; which was used by thc ancienrs fo r it's
fertility and happiness. Named after briniant magieal ap hrodesiac properties probably cho-
16th c. ruler of Iran . sen for it's shapc, ra thcr than drug concento
 Rack cOller "Thc Coming of Age Initiation":
Diegueiio Indian Sand Painting, M e ~:l Grande,
San Diego COLln ty , California . Ncar the Spring
equi no:\:, this sand painting functioned as thc
focal point for pubcrty rituals of the young
pcoplc of thc meS:l. Thc ritllal \Vas origina li)'
:ln:ompanicd by use of a vision-producing
wecd in a drink, but this praeticc was somc-
times ia tal tu the initiatc :md \Vas thcrcforc
ab:mdoncd.

J)csigllct! by E)c Wr:l)'