温和催化液相重排制备ε-己内酰胺

facile Beckmann rearrangement to ε-caprolactam in liquid phase

摘要:

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，具体为：环己酮肟2.0g，对甲苯磺酰氯1.5g，乙腈20mL，反应温度60℃，反应时间2.5h。该方法反应条件温和，操作简单，溶剂乙腈可重复使用，在较佳的条件下，环己酮肟转化率达98.4%，ε-己内酰胺选择性达93.6%。

Abstract:

The liquid-phase Beckman rearrangement of cyclohexanone oxime to ε-caprolactam with TsCl(p-toluenesulfonyl chloride) as catalyst and acetonitrile as solvent has been studied. The effects of catalyst, reaction temperature, reaction time, the dosage of catalyst, the amount of catalyst on the yield of ε-caprolactam were investigated. Under the optimized reaction conditions, cyclohexanone oxime 2.0g, TsCl 1.5g, solvent acetonitrile 20mL, reaction temperature 60℃, reaction time 2.5h, The conversion of oxime and the selectivity to ε-caprolactam were 98.4% and 93.6%, respectively. This method has an advantage of mild reaction conditions and Solvent acetonitrile can be reused.