Degradation of N,N′-dialkyldiazenedicarboxamides with a copper(II) reagent, which was prepared from lithium 4-nitrophenoxide and copper(II) bromide in tetrahydrofuran, proceeded via formation of isocyanate to produce the corresponding 4-nitrophenyl N-alkylcarbamate with the evolution of nitrogen. Further, it was also found that 4-nitrophenyl N-alkylcarbamate reacted with primary or secondary amines