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以对甲苯磺酰氯(TsCl)作催化剂,乙腈为溶剂,催化环己酮肟液相贝克曼重排制备ε-己内酰胺。考察了不同的催化体系、反应温度、反应时间、催化剂用量、溶剂用量等因素对反应的影响,建立了适宜的反应条件:环己酮肟2.0 g,对甲苯磺酰氯1.5 g,乙腈20 mL,反应温度60℃,反应时间2.5 h,环己酮肟转化率达98.4%,ε-己内酰胺选择性达93.6%。该法反应条件温和,操作简单,溶剂乙腈可重复使用。
Using t-toluenesulfonyl chloride (TsCl) as catalyst and acetonitrile as solvent, Beckmann rearrangement of cyclohexanone oxime was performed to prepare ε-caprolactam. The effects of different catalytic systems, reaction temperature, reaction time, amount of catalyst and solvent on the reaction were investigated. The optimum reaction conditions were as follows: cyclohexanone oxime 2.0 g, p-toluenesulfonyl chloride 1.5 g, acetonitrile 20 mL, The reaction temperature was 60 ℃, the reaction time was 2.5 h, the conversion of cyclohexanone oxime was 98.4% and the selectivity of ε-caprolactam was 93.6%. The reaction conditions mild, simple, solvent acetonitrile can be reused.