The perfluoroalkylthiolation reaction of indoles with perfluoroalkanesulfenic acids was achieved under mild conditions, while CH3COOH or TfOH was used as additive to promote the perfluoroalkylthiolation of activated benzene and pyrrole derivatives. A series of perfluoroalkylthiolated benzenes and heteroaromatic compounds were synthesized in moderate to good yields under transition‐metal‐free conditions.
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