Analytical

Discover Coolmate

Low temperature Microwave Synthesis System

 

Discover Coolmate can perform low- to room-temperature reactions in a microwave synthesis system and still achieve the same rate enhancements commonly associated with high-temperature reactions. The new Discover CoolMate System performs standard temperature-sensitive reactions including formation of carbanions and other highly reactive intermediates,

as well as carbohydrate chemistry, while giving you the security of knowing that your reactions are under constant temperature control. The system is also ideal for the safe use of highly reactive species in a microwave system, an area previously considered beyond the reach of microwave-enhanced synthesis.

  • Integrated cooling system assures the lowest temperature range possible with any microwave system
  • Jacketed vessel design with removable reaction vials for convenience and easy setup
  • Exclusive microwave-transparent cooling media
  • Work with reaction volumes from 500 μL –to 6 mL
  • Measure actual reaction temperature with in situ fiber optic probe
  • Onboard reaction monitoring provides feedback for unattended operation

 

CoolMate gives chemists access to new pathways in temperature-sensitive reactions, some of which cannot be produced under conventional conditions. Because microwave energy is transferred kinetically, not thermally, microwaves can accelerate reactions maintained at low temperatures. CoolMate’s proprietary, jacketed reaction vessel and exclusive cooling media are both microwave transparent, insuring the full energy transmission directly to your reactants. The

vessel and cooling technology keep the bulk temperature of the reactants low, preventing thermal degradation of the product. Temperature measurement is accomplished with an in situ fiber-optic probe to insure fast, accurate and convenient reaction control.

The cis isomer is the desired product in the substitution reaction between cis-1,4-dichloro-2-butene and a phenoxide anion in Figure 1. Conventionally, this reaction takes 21 hours. It is held for 6 hours at 0°C, then it is allowed to warm to 20 °C and react for an additional 15 hours. Using CoolMate, CEM Chemists were able to accelerate the reaction by allowing it to proceed for 35 minutes at 30 °C. The microwave procedure achieved an 87% yield, favorably compared to the 75% yield conventionally. The formation of the cis isomer was confirmed.

Elimination reactions catalyzed by n-butyllithium typically necessitate room temperature, or lower, reaction conditions. Previously, these temperature limits prevented its use in a microwave. The reaction shown in Figure 2 illustrates how a reactive species, such as n-butyllithium, can be utilized in a microwave. To achieve a 78% yield conventionally, the reaction took 2.5 hours, ranging in temperature from 0 °C to 25 °C. Because the transfer of energy in a microwave is dependent on kinetic transfers and not on thermal energy, the transformation could be accomplished at –60 °C in 5 minutes with a yield of 81%.

The versatile Discover platform, CoolMate offers all of the ease-of-use and flexibility for which CEM Life Science systems are known, including fiber optic direct temperature measurement, complete programmable control of power and temperature, and the ability to use additional standard glassware. Intuitive software enables simple translation of conventional methods to microwave conditions and the robust, compact system fits into a standard fume hood.

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