Direct Oxidative Disulfenylation/Cyclization of 2′‐Hydroxyacetophenones with Thiophenols for the Synthesis of 2,2‐Dithio‐Benzofuran‐3(2 H )‐Ones

A direct oxidative disulfenylation/cyclization of 2′‐hydroxyacetophenones with thiophenols mediated by TBAI/K 2 S 2 O 8 has been successfully developed within this study. The reaction successfully provides an efficient method for the synthesis of functionalized 2,2‐dithio‐benzofuran‐3(2 H )‐ones, which exhibits readily available starting materials, a broad substrate scope, excellent yields, and large‐scale applicability. In a single step, two C−S bonds and one C−O bond are simultaneously built on the same sp 3 carbon atom under transition‐metal‐free conditions.