Ketone derivatives are pivotal intermediates in pharmaceutical synthesis, yet conventional syntheses often rely on metals, high temperatures, and prolonged reaction times. Herein, we report a metal‐ and oxidant‐free electrochemical decarboxylative coupling of alkyl carboxylic acids with vinyl azides. The reaction proceeds sustainably in aqueous acetonitrile through a proton‐coupled electron transfer, generating NH imines that undergo in situ hydrolysis to afford ketones. The concise synthesis of Fenbufen exemplifies the green character of this radical‐based transformation.
Li et al. (2026) studied this question.