Microwave Synthesis Solutions

::: Excellence in Microwave Synthesis

The Complete Family:

Microwave Synthesis
Since its beginning in 1986, microwave synthesis has successfully matured, particularly within the last decade. All the while, Anton Paar has continuously designed and introduced reliable and versatile microwave instrumentation that fulfils the requirements of modern academic and industrial research. The new generation of Anton Paar microwave synthesis solutions is developed in response to the increasing demand , particularly in the pharmaceutical industry, for straight-foward solutions that cover the entire range of microwave synthesis applications: from initial R&D to kilolab processing.

The key: Direct scalability Method transfer from the development stage to larger quantities is a major concern in microwave synthesis. As no microwave effects are involved, the reliability of a method solely depends on the temperature measurement. Accurate internal temperature measurement and the resulting knowledge about the real reaction temperature is the key issue for successful scale-up. Once the reaction temperature is known, an optimized protocol can be applied in any suitable scale without losing efficiency.

Serving your needs in drug discovery From smallest quantities to gram-scale library generation and multigram batch processing the initial steps of the drug development process are completely covered by the members of the Anton Paar microwave synthesis product family. You can be sure to find the right solution for your specific application.

Any chemistry, any scale, anyone, anywhere!

Getting started Method development with Monowave 300 opens up pathways to new reaction routes for a broad variety of applications. Sequential method optimization employing MAS 24 with Monowave 300 or parallel optimization with the silicon carbide rotors of Synthos 3000 considerably facilitates chemists everyday work.

Want more? For parallel scale-up to the multigram range, use Rotor 16. Direct scalability of your optimized methods allows for library generation in significant gram amounts. Looking for extremes? The combination of Synthos 3000 and its Rotor 8S is the proper choice.

The big deal! Batch-type processing in the liter scale with Masterwave BTR leads to as much as 250 g product in a single run. The identical software user interface allows direct method transfer from Monowave 300. Simply multiply the amounts of your mixture and follow your optimized protocols.

New Dimensions for R&D Monowave 300

The Monowave 300 monomode microwave reactor provides a completely new and sophisticated approach towards microwave synthesis, turning previously unachievable reliability and performance into threedimensional fact. Extended operation limits up to 300 C and 30 bar (435 psi) provided by a single 850 W magnetron open up unforeseen opportunities for method development and optimization.
Reliable mate Monowave 300 your trustworthy workhorse in student education, pharmaceutical research, material science, polymer chemistry and much more opens up pathways to new reaction routes for a broad variety of applications. Reliability, scalability and reproducibility are proven in great detail.

Serving individual needs Different reaction vials provide access to various scales from 0.5 mL to 20 mL reaction volume. There is no hassle with varying caps one size fits all vials. In addition, the extended reusability of all items keeps running costs low. Even harsh and tricky chemistry involving corrosive reagents or low absorbing solvents is easily performed. A special 10 mL reaction vessel made of silicon carbide allows for trouble-free processing and even supports investigations into microwave effects.

Accurate process control Monowave 300s immersing ruby-based fiber optic sensor ensures immediate feedback, approaching the peak of precision in temperature measurement. Accurate knowledge of reaction temperature is the key factor for efficient, successful scale-up.

Seamless Automation MAS 24

The MAS 24 autosampler unit for Monowave 300 provides reliable unattended sequential operation. Up to 24 vials of different size are easily queued and processed automatically. The smart software-guided loading strategy in combination with a separate vial insert and handling position prevents sample mix-ups. Any basic Monowave 300 reactor is easily upgraded to an automated version.

Take home your advantage 4 Rapid and uniform heating 4 Utmost accuracy and reproducibility 4 New dimensions of method development & optimization 4 Simultaneous internal & IR temperature measurement 4 Powerful stirring for optimized agitation 4 Built-in touchscreen controller 4 User-friendly intuitive software 4 Durable & reusable vials, caps and septa 4 Minimum lab space required 4 Dependable gripper driven by compressed air 4 Different carousels with maximum capacity 4 Comprehensive data management

Applicable vial types

Carousel types for MAS 24

Scale Out and Prosper Synthos 3000

The Synthos 3000 multimode microwave reaction system has been developed to enhance the performance of microwave-assisted synthesis. Two magnetrons provide 1400 W unpulsed microwave output power for uniform heating. The systems installation-free wireless sensor technology facilitates handling and optimizes reaction control, leading to highly reproducible results.

Valued versatility The versatile Synthos 3000 platform provides small-scale highthroughput rotors for parallel optimizations and library generation as well as large-scale rotors for multigram parallel synthesis. The systems proven scalability ensures seamless scale-up from the milligram to the multigram range without changing instruments. Exceptional reaction conditions allow users to establish completely new reaction pathways, including near-critical water conditions. With a simple rotor switch, the scope of your microwave synthesis is easily extended.

Rotor type Reaction container Reaction volume Max. temperature Max. pressure

4x48MC Well Plate 6x8 SiC microtiter plate 0.1 0.3 mL 200 C 20 bar

4x20MGC HPLC/GC vial in 5x4 SiC plate 0.1 1.5 mL 200 C 20 bar

4x24MG5 Glass vial in 6x4 SiC plate 0.3 - 3.0 mL 200 C 20 bar

64MG5 Glass vial 0.3 - 3.0 mL 200 C 20 bar

Parallel Synthesis
The perfect match Thorough investigations and exceptional design lead to a family of small-scale rotors for Synthos 3000 that perfectly match the requirements for microwave-assisted parallel synthesis in a combinatorial manner. The silicon carbide employed in Rotor 4x48MC Well Plate, Rotor 4x20MGC and Rotor 4x24MG5 opens extraordinary avenues for method development. Being an excellent microwave absorber, SiC allows the use of any kind of solvent for microwave synthesis. In fact, virtually microwavetransparent compounds such as toluene or dioxane can be heated rapidly in SiC plates. This small-scale high-throughput equipment is especially useful for applications related to the drug development process, forensics, proteomics and other research areas which predominantly deal with small sample quantities.

Rotor types for reaction screening and parallel optimization

Various types of available SiC plates

Scale Up and Explore Synthos 3000

Synthos 3000 already provides certain scalability within its various rotor types. All methods developed in the small-scale rotors can be applied in the high-performance rotors with their 100 mL reaction vessels. The different rotor and vessel types provide the best solutions for your individual experimental tasks. Multigram parallel synthesis as well as parallel batch processing are served in all high-performance rotors. The vessels and pressure jackets are easily Interchangeable, allowing for simple upgrade to a high-pressure configuration at any time.

Anything special? Benefit from a variety of Synthos 3000 accessories: With the sophisticated gas loading system, a reactive or inert gas atmosphere is individually created in each vessel. Pressures up to 20 bar can be applied prior to reactions for safe and effective syntheses employing sensitive substrates. Utilizing standard HPLC/GC vials as proper inserts for the 100 mL vessels enables protein hydrolysis in mg quantities in a high-throughput manner. Thick-walled quartz vessels enable conditions up to 300 C and 80 bar and are even suitable for hydrothermal nanomaterial synthesis and near-critical water chemistry. Even photochemistry applications can be served with microwave-induced UV lamps.

Rotor type Reaction vessel Reaction volume Pressure jacket Max. temperature Max. pressure

48MF50 50 mL PFA 6 - 25 mL PEEK 200 C 20 bar

16MF100 100 mL PTFE-TFM 6 - 60 mL PEEK 200 C 20 bar

16HF100 100 mL PTFE-TFM 6 - 60 mL Ceramic 240 C 40 bar

8SXF100 100 mL PTFE-TFM 6 - 60 mL Ceramic 260 C 60 bar

8SXQ80 80 mL Quartz 6 - 60 mL n/a 300 C 80 bar

High-performance Synthesis
Features & benefits 4 Reliable temperature and pressure sensors optimized reaction control 4 Installation-free remote sensor technology easy handling, wireless data transmission 4 Applied silicon carbide technology efficient, homogeneous heating of small quantities 4 Sophisticated accessory simplified advanced processing 4 Highest accessible reaction conditions extending the scope of microwave synthesis 4 Multiple safety system safe, trouble-free processing at extreme conditions

All-purpose setup The individual parallel synthesis rotors for Synthos 3000 are your reliable partners in drug discovery, biomedical sciences, nanomaterial research, forensic medicine and much more. The basic Synthos 3000 instrument hosts all rotor types. Once the system is installed in your lab, future upgrades are possible at any time.

Easy-handling gas loading system

Microwave-induced UV lamps

Microwave Goes Kilolab Masterwave BTR

Based on a revolutionary new technique (patent pending, US 2009/0194528), the Masterwave benchtop reactor closes the gap between research and kilolab processing in microwave synthesis. The powerful instrument overcomes heating difficulties in scale-up and provides efficient heating and utmost productivity for a 1L reactor. Its rising-sensor temperature measurement technique provides the temperature accuracy required for direct method transfer from any smaller microwave device to the liter scale.

A kilo a day Total reaction volumes of up to 750 mL and the powerful stirrers capacity for agitating up to 200 g solid material ensures unrivaled productivity in a single run. Additionally, the instruments integrated cooling system shortens overall process times. Each reaction vessel comprises its own paddle stirrer and cap with lip-type seal. This enables you to optimize your workflow, since you can prepare the next batch while processing the batch at hand. As a result, with up to 12 subsequent cycles in a standard 8h shift, the daily production of kilogram amounts by microwave synthesis becomes a reality.

Pioneering walk on, walk off solution Despite its enhanced productivity, Masterwave BTR is still standard laboratory equipment. Placed in a regular fume hood and connected to the corresponding interfaces, any chemistry can be started right away. No specific safety measures have to be observed, no extraordinary pre-installation measures are required simply use the available lab space in the most efficient way. For your convenience, processing can also be controlled via an optional remote control from any desktop PC.

A New Dimension in Microwave Synthesis

Pushing technical frontiers 4 1700 W applicable microwave power 4 Reaction conditions up to 250 C and 30 bar 4 Rising Pt100 sensor for internal temperature measurement 4 Sliding cover with embedded hydraulic pressure sensor 4 Bayonet-locked 1 L PTFE reaction vessel 4 Vessel-integrated magnetically driven paddle stirrer 4 Internal closed-cycle cooling system 4 Compressed-air-driven vessel ejector

Microwave synthesis excels in: 4 Method development, optimization, and scale-up 4 Building block synthesis 4 Scaffold decoration 4 Metal-catalyzed reactions 4 Preparation of nanoparticles 4 Hydrothermal zeolite synthesis 4 Solid-phase reactions 4 Polymer synthesis 4 Ionic liquid chemistry

1 L PTFE reaction vessel with integrated paddle stirrer

Inserting the vessel

Fotos: Croce & Wir

Anton Paar GmbH Anton-Paar-Str. 20 A-8054 Graz Austria - Europe Tel: +43 (0)316 257-0 Fax: +43 (0)316 257-257 E-mail: [email protected] Web: www.anton-paar.com

Instruments for: Density & concentration measurement Rheometry & viscometry Sample preparation Microwave synthesis Colloid science X-ray structure analysis Refractometry Polarimetry High-precision temperature measurement Specifications subject to change without notice. 02/11 XCAIP014EN-A