N,N'-二环己基二氮烯-N,N'-二氧化物的合成

研究了用组合氧化剂过碳酸钠-过氧化氢-四乙酰乙二胺氧化环己胺制备N,N'-二环己基二氮烯-N,N'-二氧化物,通过正交实验、单因素实验考察了氧化剂各成分投料比、pH、反应温度、反应时间及反应后陈化时间对产物收率的影响.优化的工艺条件为n(环己胺):n(过碳酸钠):n(H2O2):n(四乙酰乙二胺)=1.0:3.0:3....

Synthesis of N,N'-dicyclohexyl-diazen-N,N'-dioxide

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.