A simple and metal‐free perfluoroalkylation of 4‐quinolones have been developed using sodium perfluoroalkyl sulfinates and ammonium peroxodisulfate in DMSO under mild conditions. This transformation provides direct access to C‐3 perfluoroalkylated 4‐quinolones with broad functionality in satisfactory yields. The control experimental results suggest a radical mechanistic pathway was involved in this protocol.
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