We describe a decarboxylative coupling reaction of N‐hydroxyphthalimide esters with bromopolyfluorobenzene enabled by the synergetic action of Hantzsch ester, photoredox catalyst, and nickel catalyst. This method readily converts primary and secondary alkyl carboxylic acids into the corresponding polyfluoroaryl compounds with broad scope and excellent functional group compatibility. The practicality of this method was further demonstrated by the direct modification of amino acids and biologically active molecules
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