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Enhanced Microwave-Assisted Synthesis Synthos 3000

With the Synthos 3000 multimode microwave reactor Anton Paar offers an instrument dedicated to microwave-assisted organic synthesis (MAOS), serving special features for scaling up various organic syntheses at high temperatures and high pressure, even in a combinatorial approach. Additionally available accessories make the Synthos 3000 a powerful tool for microwave-assisted chemistry, supporting several common laboratory methods in research and production as well as new reaction avenues in method development.

The Synthos 3000 enables direct scalability of well-established small-scale synthesis protocols into the multi-gram scale of products within one run, offering parallel rotors with 8, 16 or 48 vessels. The highly homogeneous microwave field allows for elaboration of reactions in parallel matter for up to 48 different mixtures in one rotor. The 16-position rotor is the universal tool for MAOS under standard microwave conditions (up to 240 °C, 40 bar), whereas Rotor 8 allows you to employ extreme temperature/pressure conditions (up to 300 °C, 80 bar). The high-throughput Rotor 48MF50 is specially designed for the library generation of valuable targets in gram scale.

Features & Accessories
Due to the highly homogeneous microwave field, provided by two magnetrons, uniformity during the reaction progress is ensured, leading to excellent reproducibility. Wireless temperature control is conducted by a gas balloon thermometer immersed in one reference vessel. As an additional control system an IR sensor measures the temperature on the outer surface of any vessel from the bottom of the cavity. The built-in magnetic stirrer can further enhance reaction rates, especially when inhomogeneous mixtures are heated.

Pressure measurement is achieved simultaneously for all vessels (Rotor 8) by a unique hydraulic pressure system integrated in the rotor top plate. With Rotor 16 and Rotor 48, parameter control is accomplished by a combined pressure/temperature sensor immersed in one reference vessel.

The maximum output power of 1400 W allows efficient heating rates with even large amounts of reaction mixtures. Cooling is achieved by a forced-air cooling system, which can decrease the temperature from 280 °C to ~40 °C within 20-30 minutes.

The high-throughput Rotor 48 can be equipped with up to 48 reaction vessels arranged in three circles. Each reaction vessel consists of a 50 mL PFA liner, a pressure jacket and a screw cap containing a cone seal for quick and safe handling. Reaction control is achieved on the center circle by IR control and more precisely by an immersing temperature/pressure sensor in one reference vessel. Even small amounts, such as only 4 mL in a single vessel, can be processed effectively in an operation range of up to 200 °C and 20 bar. Therefore, the Rotor 48MF50 is highly applicable not only for scaling up parallel synthesis of various derivatives but also for method development.

The standard vessels of Rotor 8 and Rotor 16 are made of a 100 mL PTFE liner immersed into a pressure jacket. Different materials of these jackets allow for operation limits up to 260 °C and 60 bar at a volume of 6-60 mL per vessel. The special 80 mL quartz vessels for Rotor 8 offer an operating range up to 300 °C with a maximum working pressure of 80 bar. With this equipment even near critical water chemistry can be carried out easily and safely. Hermetic lip-type sealing prevents loss of volatile compounds when carrying out reactions high above the boiling points of used solvents.

To simplify washing and cleaving steps in solid phase synthesis under microwave conditions, a special filter unit for the 100 mL vessels is available. This tool can be applied directly on the non-adhesive PTFE-TFM liners in order to carry out a whole SPOS reaction sequence without changing the vessels.

An additional gas inlet system for use with the Rotor 8 and Rotor 16 allows you to apply individual pre-pressures of up to 20 bar with either reactant or inert gas atmospheres. This simplifies the handling of air/moisture-sensitive reagents while combining the benefits of microwave heating with the effects of high-pressure conditions.

For effective heating of weakly absorbing agents, inert passive heating elements made of silicone carbide (SiC), are available. These re-useable tools enable transformations in non-polar solvents at much higher temperatures than could be usually reached by microwave irradiation.

The delivered software package provides a common solvent/reactant library for easy generation of new reaction protocols. Several standard protocols for frequently used reactions are included which can be edited for your individual needs.

Safety Aspects
The Synthos 3000 guarantees the highest safety standards serving various active and passive safety measures to protect users against hazards from unexpected spontaneous chemical reactions.

To protect the vessels from damage, they are equipped with metal safety disks which open in case of sudden overpressure formation. In case of a venting action, the overpressure is released by a quick opening and immediate resealing of the cavity door.

Furthermore, the software controls the microwave output by switching off the magnetron and starting the cooling system if the temperature or pressure increase exceeds the safety limit. The magnetron is protected against overheating due to reflected irradiation by an accurate double-check temperature control system.

For further information about microwave-assisted synthesis with the Synthos 3000 from Anton Paar, please take a look at our product brochure (PDF file)