Abstract The electrochemical synthesis of the 2‐arylpropionic acid group of nonsteroidal anti‐inflammatory agents such as ibuprofen, naproxen, indoprofen, biprofen, cicloprofen, and fenoprofen has been carried out in dimethylformamide (DMF) containing tetra‐n‐butylammonium perchlorate (nBu4NClO4) by electrochemical carboxylation of α‐methylbenzyl chlorides catalyzed by a schiff‐base complex [Co(salen)] in an undivided cell equipped with a platinum cathode and magnesium anode under constant current density of 10 mA/cm2 in good yields. Cyclic voltammetric studies have also been carried out to investigate the mechanism by which [Co(salen)] catalyzes the cathodic reaction of α‐methylbenzyl chlorides in presence of CO2 by taking α‐phenylethylchloride as the model compound. Keywords: Benzyl chloridecarbon dioxidecarboxylic acidcobalt complexcyclic voltammetry Acknowledgments J.D. is thankful to Council of Scientific and Industrial Reseacrh, New Delhi, India, for providing financial assistance in the form of a Senior Research Fellowship.