A low-volume flow electrochemical microreactor for rapid and automated process optimization

Electrochemical reactions under constant current can be completed within very short periods of time in microliter-volume cells, as electrolysis time is proportional to the quantity of material processed. A flexible electrochemical microreactor with 17 mu L volume has been designed and constructed, which enables reactions to be performed in as little as 7.3 s residence time using standard, commercially available electrodes. By utilizing automation and statistical analysis, the reaction design space was explored for three model reactions in 2-3 hours, consuming only 30-300 mg of material for 42 experiments. A microliter-volume flow electrolysis cell, combined with a fully automated platform which includes parameters variation and sample collection, enables high-throughput screening of electrolysis conditions within 2-3 hours.