Reduction of 2,3-dimethyl-2,3-dinitrobutane with Zn in aqueous ethanol in the presence of NH(4)Cl affords 2,3-bis(hydroxylamino)-2,3-dimethylbutane together with 2,3-diamino-2,3-dimethylbutane and complex Zn salts. A modified procedure was developed for the synthesis of bishydroxylamine, which involves reduction in a Zn/NH(4)Cl/THF-H(2)O system.