A green electrochemical method of preparing diacid-disulfides has been developed, in which an SÀ S bond is formed by electrochemically oxidative coupling of SÀ H/SÀ H employing redox active NaI as mediator. The reactions are carried out in a simple undivided cell under constant current condition at room temperature and complete in 1.3 h to afford a series of diaciddisulfides with up to 97 % yields.
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