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Activation of two sp 3 -C-H bonds and oxidative alkylation of sp 3 -C-H bond adjacent to a nitrogen atom of tertiary amine were catalyzed by Bu 4 NAuCl 4 with H 2 O 2 as oxidant under mild reaction conditions. The safe, convenient, and environmentally benign process, as well as the broad substrate scope, low catalyst loading, high selectivity, short reaction time, and good yields make the protocol very practical.doi:10.6023/cjoc201210029 fatcat:qwnmibgfcvblfdt7x3gdkqajky