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The sulfenylation of the vinyl C-H bond in ketene dithioacetals leading to the synthesis of polythiolated alkenes is achieved via the promotion of molecular iodine. In addition, alkyl thiols also exhibit tolerance to the C-H bond elaboration reaction for the synthesis of corresponding alkylthiolated ketene dithioacetals.

Metal-Free Vinyl C–H Sulfenylation/Alkyl Thiolation of Ketene Dithioacetals for the Synthesis of Polythiolated Alkenes