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The synthesis of chiral tetrahydrofurans and pyrrolidines starting from 1,2‐diols or β‐amino alcohols, respectively, by visible‐light‐mediated deoxygenation is described. Easily accessible monoallylated/propargylated substrates were activated either as inexpensive ethyl oxalates or as recyclable 3,5‐bis(trifluoromethyl)benzoates to generate alkyl radicals suitable for 5‐ exo ‐ trig /5‐ exo ‐ dig  cyclizations under visible‐light irradiation.

Synthesis of Chiral Tetrahydrofurans and Pyrrolidines by Visible‐Light‐Mediated Deoxygenation