Scaling-up Electroorganic Synthesis Using a Spinning Electrode Electrochemical Reactor in Batch and Flow Mode

Abstract

Technology for the rapid scale-up of synthetic organic electrochemistry from milligrams to multigrams or multi-100 g quantities is highly desirable. Traditional parallel plate flow electrolysis cells can produce large quantities of material, but transfer from batch to this flow technology requires reoptimization of the reaction conditions and fully homogeneous reaction mixtures. Moreover, single-pass processing is often difficult to accomplish due to gas generation and the low flow rates typically used in continuous mode. Herein we present a novel reactor design, based on a rotating cylinder electrode concept, that enables seamless scale up from small scale batch experimentation to gram and even multikilogram per day quantities. The device can operate in batch and flow mode, and it is able to easily process slurries without clogging of the system or fouling of the electrodes. Continuous operation is also demonstrated using three reactors in series that act as a continuous stirred electrochemical reactor cascade, providing kilogram per day productivities in a single pass.