A direct one-pot alkylation-aminoxidation of styrene derivatives was achieved using -generated alkyl and -oxyl radicals. The corresponding -alkylated hydroxylamine derivatives were obtained in moderate to good yields. The reaction features the generation of the alkyl radicals from phenyliodine(III) dicarboxylates an organocatalytic process, the use of phenyliodine(III) dicarboxylates as the source of the alkyl radicals and oxidants for the generation of -oxyl radicals, and the first generation of the β-enaminyl radicals a HAT process and their use as single-electron donors.

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