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A visible‐light mediated exclusively regioselective synthesis of 2,2‐disubstituted thio‐functionalized tetrahydrofurans, tetrahydro‐ pyrans and oxepanes has been described through an operationally simple and mild photoredox protocol. Thiyl radical generated from N‐phenylsulfenyl phthalimide by photoredox catalysis was proven to be the key reactive intermediate in this reaction.
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