温和催化液相重排制备ε-己内酰胺  

Facile Beckmann Rearrangement to Synthesize ε-Caprolactam in Liquid Phase

作　　者：张风雷[1] 章亚东[1] 

机构地区：[1]郑州大学化工与能源学院,河南郑州450001

出　　处：《精细化工》2013年第9期1073-1076,共4页Fine Chemicals

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: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。The liquid-phase Beckmann rearrangement of cyclohexanone oxime to synthesize 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, and the amount of solvent on the yield of ε-eaprolactam were investigated. Under the optimized reaction conditions of eyclohexanone oxime 2.0 g, TsCl 1.5 g, solvent acetonitrile 20 mL, reaction temperature 60℃, and reaction time 2.5 h, the conversion of oxime and the selectivity of ε-caprolactam were 98.4% and 93.6%, respectively. This method has the advantages of easy operation, mild reaction conditions and the reusability of the solvent acetonitrile.

关 键 词：对甲苯磺酰氯 己内酰胺 贝克曼重排 精细化工中间体 

分 类 号：TQ426.94[化学工程] O623.626[理学—有机化学]