A one-step electrochemical synthesis in acetonitrile or dimethyformamide solvent, of N,O-dialkylarylhydroxylamines and N,O-diacylarylhydroxylamines, from aryl nitro compounds and alkyl halides or acyl anhydrides, was used to synthesize more than 80 new compounds. The reaction is a general reaction, tolerating most aryl substituents and most primary and secondary alkyl halides.) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 165.123.34.86