Herein, a photoinitiated radical relay reaction of quinoxalin-2(1)-ones, with acyloxy nitroso compounds as a source of radicals, is described. Although the C-H functionalization of quinoxalin-2(1)-ones has been investigated, its difunctionalization, the simultaneous construction of C-C and N-N bonds directly via the radical relay reaction, has rarely been reported. Moreover, the obtained products underwent sequential reactions to access C7-NO of quinoxalin-2(1)-ones under mild conditions.
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