Electroreductive Desulfurization of Thioacetals

A metal‐free electrochemical protocol for desulfurization of aryl thioacetals into alkanes under ambient conditions is reported. The method is fully selective for C( sp 3 )─S bond cleavage, serving as an electrochemical alternative to Mozingo reduction via intermediate formation of thioethers. With a switch of solvent, the transformation enables the formation of deuterated products.