Anodic oxidation of N (methoxycarbony1) pyrrolidines (n= 1) and-piperidines (n= 2)(A) gave a,@-disubstituted compounds B, in which the a-substituent was an acetoxy, hydroxy, or methoxy group and the@-substituent was an acetoxy group or halogen atom. The a- substituents of B were easily removed by NaBH4 under acidic conditions to give@- substituted compounds C. A reaction mechanism involving the formation of a,@- ...