ABSTRACT We report the first triple hydrogen‐atom transfer (HAT) strategy for the efficient synthesis of symmetric and asymmetric disulfides. This metal‐, oxidant‐, and solvent‐free reaction proceeds under mild conditions with excellent functional‐group tolerance and a broad substrate scope. Mechanistic studies indicate that TEMPO‐derived O‐centered radical and N‐ and O‐centered radicals formed via thiol‐assisted N–O bond cleavage engage in the triple HAT process with thiol substrates.
Liang et al. (Wed,) studied this question.