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2,2’-偶氮二(N-环己基异丁基脒)盐酸盐的合成

         

摘要

以偶氮二异丁腈为主要原料制备了2,2’-偶氮二(N-环已基异丁基脒)盐酸盐,研究了2,2’-偶氮二异丁亚胺甲醚盐酸盐及2,2’-偶氮二(N-环己基异丁基脒)盐酸盐的最佳合成工艺条件。以1,2-二氯乙烷为溶剂,n(偶氮二异丁腈):n(甲醇):n(氯化氢)=1:2.5:2.6,反应温度15-20℃,反应时间24h,得2,2’-偶氮二异丁亚胺甲醚盐酸盐,收率99.1%;以无水甲醇为溶剂,与环己胺反应合成了2,2’-偶氮二(N-环己基异丁基脒)盐酸盐,n(偶氮亚胺甲醚盐酸盐):n(环己胺)=1:2.5,反应温度30-35℃,反应时间8h,收率78.2%。产物经IR和^1HNMR等进行了确证。%2,2'- Azobis ( N - cyclohexyl - 2 - methyl propionamidine) dihydrochloride was prepared by the reaction of cyclohexylamine and azoiminoamidine hydrochloride, and the azoiminomethylether hydrochloride was prepared by azobisisobutyronitrile as the mainly starting material through Pinner reaction, the optimum condition for the preparation of the azoiminomethylether hydrochloride and 2,2'- azobis (N - eyclohexyl - 2 - methyl propionamidine ) dihydrochloride were determined; The azoiminodimethlyether hydroehloride is obtained by the molar ration n (azobisisobutyronitrile):n (methanol) : n(hydrochloride) = 1 : 2.5 : 2.6, reaction temperature 15 - 20℃ and reaction time 24h, the yield is 99.1%. Then 2,2'- Azobis ( N - cyclohexyl - 2 - methyl propionamidine) dihydrochloride was synthesized in anhydrous methanol with cyclohexylamine, n (azoiminomethylether hydrochloride ):n (eyclohexylamine) = 1:2.5, reaction temperature 30 - 35℃, and reaction time 8h, the yield was 78. 2%. The product was assignd by IR and 1H NMR.

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