The nitrolysis of N, K-disubstituted amides in trifluoroacetic anhydride has been further investigated. When the substituents are n-alkyl groups, the nitrolysis of acetamides, methanesulfonamides and benzenesulfonamides gives almost quantitative yields of the corresponding secondary nitramines. The nitrolysis, however, is retarded easily both by steric hindrance from the N-alkyl groups and by electronegative substituents.