Iodine/TBHP‐Promoted Cross Coupling of <i>N</i> ‐Hydroxy Aryl Sulfonamides and Disulfides to Synthesize Unsymmetrical Thiosulfonates

Abstract An efficient and novel method has been developed for the synthesis of structurally diverse unsymmetrical thiosulfonates via the oxidative coupling reactions of N ‐hydroxy aryl sulfonamides and disulfides. The iodine and TBHP system enables the transformations to afford a variety of thiosulfonates with good to high yields. Furthermore, the large‐scale synthesis and practical application to access sulfonamide have been investigated. Notably, the present protocol offers easily accessible materials, a wide range of substrates, radical pathways, and metal‐free conditions.