Emrys Optimizer

The Emrys Creator is the basic application tool for reactions on a 0.5-5.0 mL scale. The Emrys Optimizer allows for automation with integrated robotics so that... 

As illustrated in Scheme 1, on a small scale under reflux in ace-tone/water, 5% of starting material remained after 12 h reaction time and approximately 20% of the by-product was formed (entry 1). When performing the reaction at the same concentration in a lab-scale micro-wave device (Emrys Optimizer, entry 2) at 120°C, the reaction was complete after 5 min and gave a product of significantly higher purity and in higher yield. In the next step, 400 ml of reaction mixture was reacted in an 8 vessel rotor batch microwave (entry 3) at the same temperature... 

In various experiments, it was shown that the use of microwave technology leads to a significant decrease in the reaction time and in some cases also to less by-product and a higher yield. This technology allowed us to optimize the reaction with focus on work-up and purification, independent of reaction temperature and boiling point of the solvent. In most cases the reaction conditions, applied on 15 ml scale in the Emrys Optimizer, were transferred without further optimization to the microwave reactors tested and led to comparable results. Additional optimization in a few cases was limited to small adjustments in reaction temperature or reaction time. A number of scale-up experiments were conducted using a Synthos 3000 reactor and we showed that a scale-up to 100 g is feasible. 

Baxendale and Ley [60] employed the Smith Synthesizer as well as the Emrys Optimizer from Biotage [59] for conducting neat KOf-Bu mediated trimerizations of various liquid nitriles to give aryl- and alkyl-substituted 4-... 

Emrys Optimizer 2-5 mL pyrex reaction vessel equipped with a stir bar and purged under argon... 

To an Emrys Optimizer 2-5 mL pyrex reaction vessel Ni/C (67.3 mg, 0.04 mmol) was added under argon at room temperature. Tetrahydrofuran (1 mL) was added followed by n-BuLi (31 pL, 2.55 M in hexanes, 0.08 mmol). 

The reaction vessel was placed in the Emrys Optimizer and exposed to microwave irradiation according to the following specifications temperature 200 °C, time 600 seconds, fixed hold time on, sample absorption normal, prestirring 30 seconds. 

As a starting point for reaction optimization, Biotage offers a microwave reaction database (Emrys PathFinder) with ca. 4000 validated entries for microwave chemistry performed with Biotage single-mode instruments. 

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