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We developed a novel and efficient method for the synthesis of various 3‐alkylated quinoxalin‐2(1H)‐ones (32 examples, 70%–96% yields) through electron donor‐acceptor complex enabled alkylation of quinoxalin‐2(1H)‐ones with N‐ hydroxyphthalimide esters as the alkyl source and Na2S as the catalytic electron donor under external photocatalyst‐, oxidant‐ and additive‐free conditions. Various 3‐alkylated quinoxalin‐2(1H)‐oneswere synthesized through electron donor‐acceptor complex enabled alkylation of quinoxalin‐2(1H)‐ones with N‐hydroxyphthalimide esters (alkyl source) and Na2S (catalytic electron donor) under external photocatalyst‐, oxidant‐ and additive‐free conditions.

A novel and efficient electrochemical initiated radical strategy was developed for the preparation of both N-substituted and N-unsubstituted 4-selanylisoquinolin-1(2H)-ones through selenylation of isoquinolin-1(2H)-ones with organodiselenides under chemical oxidant-, additive-free and ambient conditions.