A Continuous Flow Cell for High‐Temperature/High‐Pressure Electroorganic Synthesis.

A flow electrolysis cell that enables operation at high temperatures and pressures has been designed and developed. The cell, with a cylindrical shape and concentric electrodes, can be easily assembled using commercially available fluidic components. The compact design of the device permits easy temperature control using a commercial column heater. Temperatures ranging from −10 °C to +150 °C and pressures up to 70 bar have been successfully applied for long operation periods. The cell performance has been evaluated using the anodic methoxylation of N‐formylpiperidine as a model. Very high conversions and selectivities have been achieved with single‐pass processing, and high productivities of 73 mmol/h with electrolyte recycling. The high pressure and temperature capabilities of the cell have been used to demonstrate the negative effect that re‐dissolved hydrogen gas can have on hydrogen‐releasing electrochemical reactions in undivided cells, owing to undesired anodic oxidation of hydrogen. [ABSTRACT FROM AUTHOR]