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    Dimethylamine PDF

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    angelofglory
    The document discusses several methods for synthesizing dimethylamine, including: 1. Refluxing DMF with HCl for over 6 hours and doing an acid/base extraction. 2. Reacting methylamine HCl with formaldehyde between 105-115°C for a few hours. 3. Heating a mixture of ammonium chloride, formalin, and water at specific temperatures over time, then extracting with chloroform or DCM.

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    Dimethylamine PDF

    Uploaded by

    angelofglory
    212 views2 pages
    The document discusses several methods for synthesizing dimethylamine, including: 1. Refluxing DMF with HCl for over 6 hours and doing an acid/base extraction. 2. Reacting methylamine HCl with formaldehyde between 105-115°C for a few hours. 3. Heating a mixture of ammonium chloride, formalin, and water at specific temperatures over time, then extracting with chloroform or DCM.

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    The document discusses several methods for synthesizing dimethylamine, including: 1. Refluxing DMF with HCl for over 6 hours and doing an acid/base extraction. 2. Reacting methylamine HCl with formaldehyde between 105-115°C for a few hours. 3. Heating a mixture of ammonium chloride, formalin, and water at specific temperatures over time, then extracting with chloroform or DCM.

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    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    212 views2 pages

    Dimethylamine PDF

    Uploaded by

    angelofglory
    The document discusses several methods for synthesizing dimethylamine, including: 1. Refluxing DMF with HCl for over 6 hours and doing an acid/base extraction. 2. Reacting methylamine HCl with formaldehyde between 105-115°C for a few hours. 3. Heating a mixture of ammonium chloride, formalin, and water at specific temperatures over time, then extracting with chloroform or DCM.

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    of 2

    search the Hiveboard, powered by sphider.eu or search Rhodium's PDF, powered by freefind.

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    Ghost_Of_BT Dimethylamine synth


    (Hive Bee)
    09-13-01 23:27 There was a process given on Rhodium's page where dimethylamine is synthesized by refluxing DMF with HCl for
    No 213225 over 6h and doing an a/b extraction. However, in Rhodiums Methylamine FAQ, another synthesis is given. Simply
    react methylamine HCl with formaldehyde. Now doesn't that sound better? My question is how I should go about
    doing this. Could I just boil methylamine HCl in an access of paraformaldehyde in water above 115deg for a few
    hours? What would you suggest? Here's the section from Rhodium's FAQ:

    Methylamine hydrochloride condenses with formaldehyde to form dimethylamine. If formaldehyde is present in


    excess, at least some of the methylamine is converted to dimethylamine. If too little formaldehyde is present, the
    methyleneimine polymerizes to its trimer, (CH2=NH)3. Trimethylamine is never formed, as long as the temperature of
    the solution never exceeds 110°C. With an excess (4 moles) of formaldehyde, enough water and a reflux
    temperature of 115°C, dimethylamine is the main product, as the temperature rises, more dimethylamine is formed.
    Dry heating of paraformaldehyde and ammonium chloride produces trimethylamine through reaction of dimethylamine
    with formaldehyde, giving rise to tetramethylmethylenediamine and formic acid, and the base further reacts with
    HCl, giving trimethylamine hydrochloride and methyleneimine hydrochloride. A mixture of HMTA and HCl boils between
    105 and 110°C, while NH4Cl/CH2O boils at 115°C. No temperature control is really necessary in the former case, as
    long as your heating plate isn't too hot. If the reaction is carried out at a lower temperature, less dimethylamine is
    formed, and the yield is higher. Vacuum reflux and distillation can yield at least 95% yield, in contrast to the 45%
    gotten at 104°C.

    terbium Re: Dimethylamine synth


    (Old P2P Cook)
    09-14-01 07:03 From Vogel:
    No 213378 Proceed as in the preparation of methylamine hydrochloride Post 209576 (terbium: "Re: Methylamine; So many
    problems? Is it the Altitude", Newbee Forum) using 200 gram of ammonium chloride and 400 gram of formalin, and
    heat the mixture at 104°C until no more fluid distills. Cool to room temperature and filter off the ammonium chloride
    (ca. 50 g): add 300 g. of formalin to the filtrate, return the solution to the distilling flask, heat until the temperature
    reaches 115°C and maintain it as nearly as possible at this temperature until no more liquid passes over (about 3-4
    hours). Concentrate the residue in the distilling flask on a water bath until a scum appears on the surface of the
    hot liquid. Cool to room temperature and filter off the solid (ca. 32 g.; impure methylamine hydrochloride containing
    about 25% of ammonium chloride). Pour back the filtrate into the distilling flask and heat to 120°C until a sample of
    the liquid, on cooling, becomes semi-solid. Transfer it to a vacuum desiccator charged with sodium hydroxide pellets
    and leave it there for 2 days. extract the residue with hot chloroform and filter; on cooling, crystals of
    dimethylamine hydrochloride separate. A further crop can be obtained by evaporating the filtrate to about half its
    original volume. The yield is 120 g.

    Ghost_Of_BT Re: Dimethylamine synth


    (Hive Bee)
    09-14-01 18:14 Thanks! Surley the vacuum desicator can be removed from the proceedure and perhaps DCM can replace
    No 213530 chloroform, correct?

    terbium Re: Dimethylamine synth


    (Old P2P Cook)
    09-15-01 06:38 Don't know. I would expect that, in this case, the difference in solvent properties between DCM and chloroform
    No 213770 might be significant. It may not be necessary to extract with chloroform if a product that is mostly dimethylamine
    is acceptable; a titration using a pH meter would tell you the purity of your dimethylamine.

    Ghost_Of_BT Re: Dimethylamine synth


    (Hive Bee)
    09-15-01 18:31 Or using phenothalene. I remember that stuff from chem class. You carfully add you base with stiring untill the the
    No 213842 last drop causes the solution to remain purple. Thanks again for the info. I think this is one of the only
    dimethylamine synth threads.

    halfapint Re: Dimethylamine synth


    (Ubiquitous
    Precursor Medal Spell "phenolphthalein" backwards. In case you don't want to synth dimethylamine, the weed killer (herbicide) with
    Winner) the trade name diazinon comes as the dimethylamine salt. Basify and boil it out, catch it in dilute HCl, titrate back
    09-17-01 13:10 to neutral with base, boil down to fractionally crystallize it out of the salt water. If it's still traded; herbicides and
    No 214306 insecticides have short market lives, as their specific horrors are uncovered.
    turning science fact into <<science fiction>>

    Ghost_Of_BT Re: Dimethylamine synth


    (Hive Bee)

    converted by W eb2PDFConvert.com
    09-17-01 16:57 Is it the HCl salt or what?
    No 214364

    Ghost_Of_BT Re: Dimethylamine synth


    (Hive Bee)
    09-18-01 03:41 I went to the garden store today and found several brands containing various dimethylamine salts. I bought the one
    No 214549 that was the highest in concentration and had only the dimethylamine salts as the active ingreadiants (a total of
    13%). To my delight, when I mixed a sample with NaOH, there was an obvious reaction and an ammonia smelling
    gas was produced. If this is pure DMamine gas, than one can easily make the very usefull anahydrous solution of
    DMamine in ether by simply boiling away the volitals in this stuff, mixing it with a large access of NaOH (an access
    to help absorb the water), bubble it through ether and dry over MgSO4. Could this gas possibly be anything other
    than dimethylamine? Here are the ingredients:
    Mecoprop, dimethylamine salt
    2,4-D, dimethylamine salt
    Dicamba, dimethylamine salt
    On the MSDS for this product (found on company's site), those are the only listed ingrideants so I assume the other
    86% is water.

    Vitus_Verdegast dimethylamine from hydrolysis of DMF


    (Hive Addict)
    06-16-04 01:00 To 75 g (1.03 mol) of dimethylformamide in a 500 ml roundbottom flask was slowly added, portionwise, 160 g 6N
    No 513655 aqueous hydrochloric acid. Caution, this was a very exothermic process! The flask was fit with a condensor and the
    mixture was refluxed for 7 hours. Dimethylformamide hydrolyses to dimethylamine and formic acid, so the fumes
    were led outside in case some carbon monoxide formed due to decomposition of HCOOH.

    The mixture was vacuum distilled at the fridge pump until a white mushy solid was left in the distilling flask. This
    was sucked as dry as possible on a Buchner funnel and transferred to a dessicator, where it was dried over CaCl2
    for a couple of days. There was obtained 59.3 grams of dimethylamine hydrochloride as sparkling white crystals,
    which is a yield of 70% .
    http://www.psychedelicrepublicans.com/

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