Instrumentation & Technology Overview

The CDLMC is associated with the Institute Of Chemistry at the University of Graz, Austria. Its state-of-the-art microwave reactors are used to perform a diverse range of experiments connected to both basic and applied research in the field of microwave-assisted synthesis and related areas.

 

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Available Microwave Instrumentation and Accessories

Single-Mode Microwave Reactors:

Anton Paar Monowave 300: A single-mode (850 W) microwave reactor for closed vessel synthesis up to 300 °C and 30 bar. Volumes from 2 to 20 mL can be processed using 2 different vial types. The temperature is measured simultaneously via IR and fiber-optic temperature probe.

Biotage Emrys Optimizer EXP 60: A fully automated single-mode (300 W) microwave reactor that incorporates a gripper for robotic vessel transfer of 60 microwave process vials. The system is used for the efficient optimization of reaction conditions and for the unattended generation of libraries using microwave synthesis (sealed vessels, processing volume 0.5-5 ml, max pressure 20 bar, IR temperature sensor).

Biotage Initiator EXP 8: An automated single-mode (400 W) microwave reactor that incorporates a gripper for the robotic transfer of 4 different types of sealed creation vessels allowing the processing of sample volumes from 0.2 to 20 ml (max pressure 20 bar, IR temperature sensor).

CEM Discover/Voyager: A flexible single-mode instrument (300 W) that allows batch (Discover) and continuous-flow processing (Voyager CF) and stop flow (SF) in open or sealed vessels (20 bar) up to 100 ml of volume. The system also allows the simultaneous cooling of the reaction mixture and the use of fiber-optic temperature probes.

CEM Discover SPS: A single-mode microwave reactor (300 W) for solid-phase peptide synthesis using bottom-filtration technology and fiber-optic temperature measurements.

Multimode Microwave Reactors:

 

Anton Paar Synthos 3000: A multimode microwave instrument (1400 W) dedicated for batch scale-up that allows processing of volumes of up to one liter in a variety of different rotor systems (8, 16, 48, 64). In quartz vessel rotors, processing of up to 300 °C and 80 bars is possible. The system can also be used as an autoclave using pre-pressurized and in connection with microtiter plates (gas balloon and IR temperature measurement).

Milestone MicroSYNTH Labstation: A multimode batch microwave instrument (1000 W) that allows processing of samples under open- and sealed conditions. In open vessel format several liters can be irradiated under reflux conditions. Several rotor systems are available for sealed and open vessel processing (fiber-optic and IR temperature measurement).

Additionial Instrumentation:

Flow Reactors: Thales H-Cube, X-Cube and X-Cube Flash continuous flow reactors.

HPLC: Two Shimdazu Prominence LC20A with diode array detection and autosamplers, and a Shimdazu LC10 HPLC system for semipreparative separations.

GC-MS: ThermoFisher DSQ II GC/MS with EI and CI and direct inlet probe. ThermoFisher Trace GC Ultra with FID.

Flash Chromatography: Biotage SP1 automated flash chromatography system.

The CDLMC additionally has access to various prototype microwave reactors and accessories for specific applications.

Technical Expertise at the CDLMC

  • General organic synthesis and reaction optimization under microwave conditions including DoE methods
  • Processing in open, closed and pre pressurized vessels
  • Processing under non-classical conditions and solvents (near-critical water, super-critical methanol, ionic liquids, solvent-free)
  • Specific microwave effects, accurate multiple fiber optic temperature measurements
  • Simultaneous cooling
  • Passive heating elements (silicon carbide)
  • Microwave-assisted solid-phase peptide synthesis and use of polymer-supported reagents/catalyst
  • Automated sequential or parallel processing including microtiter plate formats
  • Scale-up in batch and continuous flow reactors

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