Abstract: N,N'-dicyclohexyldiazene-N,N'-dioxide was prepared by oxidation of cyclohexylamine with the combined oxidant of sodium percarbonate-hydrogen peroxide-tetraacetylethylenediamine. Effects of the ratio of oxidant, pH, reaction temperature, reaction time and aging time after reaction on the yield were investigated by either orthogonal or single-factor experiments. The optimized process conditions are as follows: n(cyclohexylamine): n(sodium percarbonate): n(hydrogen peroxide): n(tetraacetylethylenediamine)=1:3.0:3.0:1.75, in water/ethyl acetate mixed solution (rotio of amount of substance=5.3:1.0) with pH =9 at 33 ℃ reaction for 3 h, and aging for 12 h, the yield reaches as high as 98.3%. The structure of the product was characterized by IR, ¹H NMR, ¹³C NMR and MS.

Key words: N,N'-dicyclohexyl-diazen-N, N'-dioxide, cyclohexylamine, sodium percarbonate, hydrogen peroxide, tetraacetylethylenediamine, oxidation