The intensification of electrochemical hydrocarboxylation reaction employing a spinning cylinder electrode reactor is presented. The optimized system provides high reaction scale for the synthesis of valuable compounds, incorporating CO₂ gas in organic molecules in an efficient way.

There is an increasing attention in developing reactions that can incorporate CO₂ into organic molecules. In this context, electrochemistry offers a sustainable and mild approach to utilize this valuable yet elusive C1 building block in a scalable fashion. Herein, the intensification of the electrochemical hydrocarboxylation of activated alkenes is presented. The study covers the evaluation of critical chemical and electrochemical parameters to maximize the efficiency of the process in standardized small-scale batch cells, followed by the transfer to a spinning cylinder electrochemical reactor. Leveraging the enhanced mass transfer of this reactor design, the reaction can be further optimized, leading to a more efficient process. After validating the transformation across different substrates, the regioselective addition of CO₂ is further improved by tuning the current density of the process. Finally, a scale-up in recirculation mode is performed, achieving a productivity of 55 g day⁻¹ and demonstrating its potential for the efficient and scalable utilization of the electrochemical hydrocarboxylation reaction.