合成酮麝香的重要中间体5-叔丁基间二甲苯的传统合成工艺存在酸催化剂回收利用困难、污染严重等问题。为了寻求新型绿色催化体系,合成了咪唑和季胺类功能性离子液体[Bmim]Cl-AlCl₃、[Bmim]Cl-FeCl₃、[Et₃NH]Cl-AlCl₃、[Et₃NH]Cl-FeCl₃。以[Bmim]Cl-AlCl₃离子液体为催化剂,考察了反应温度、n(间二甲苯):n(氯代叔丁烷):n(催化剂)、反应时间等对合成5-叔丁基间二甲苯的影响,并通过响应面法得出最优工艺条件:反应温度为13℃、n(间二甲苯):n(氯代叔丁烷):n(催化剂)=1:1.2:0.1、反应时间为73 min,此时5-叔丁基间二甲苯收率可达95%以上。

Traditional synthesis process for 5-tert-butyl-m-xylene,an important intermediate of ketone musk,has some problems such as difficult recovery of acid catalyst and serious pollution.In order to seek a novel green catalytic system,imidazole and quaternary amines functional ionic liquids such as[Bmim]Cl-AlCl₃,[Bmim]Cl-FeCl₃,[Et₃NH]Cl-AlCl₃,[Et₃NH]Cl-FeCl₃ are synthesized,and used to catalyze the synthesis of 5-tert-butyl-m-xylene through Friedel-Crafts alkylation reaction.Using[Bmim]Cl-AlCl₃ ionic liquid as catalyst,the influences of reaction temperature,the molar ratio of m-xylene to tert-butane chloride to catalyst,reaction time and other technological conditions on the reaction are investigated,and response surface method is used to optimize the synthesis process.The obtained optimal conditions are as follows:reaction temperature is 13℃,n(m-xylene):n(tert-butane chloride):n(catalyst)=1:1:2:0.1,and the reaction time is 73 min,under which the yield of 5-tert-butyl-m-xylene can exceed 95%.

段嘉慧(1999-),女,硕士研究生,研究方向为二氧化钛水热法合成钛酸钡,duanjiahui1114@126.com。