酸性离子液体催化合成N-氰乙基-N-羟乙基苯胺  

Synthesis of N-Cyanoethyl-N-hydroxyethylaniline Catalyzed by Acdic Ionic Liquid

作　　者：郭辉[1] 殷园园[1] 张学颖 庄玉伟[1] 曹健[1] 张国宝[1] GUO Hui;YIN Yuanyuan;ZHANG Xueying;ZHUANG Yuwei;JIAN Cao;ZHANG Guobao(High&New Technology Research Center of Henan Academy of Sciences,Zhengzhou 450002,China)

机构地区：[1]河南省科学院高新技术研究中心,郑州450002

出　　处：《应用化学》2020年第5期512-517,共6页Chinese Journal of Applied Chemistry

摘　　要：N-氰乙基-N-羟乙基苯胺是一种具有广泛用途的染料中间体,针对传统合成方法中的缺陷,以1-丁基-3-甲基咪唑硫酸氢盐([BMIM]HSO 4)为催化剂,丙烯腈和N-羟乙基苯胺为原料,建立了N-氰乙基-N-羟乙基苯胺的绿色合成新工艺。系统考察了离子液体种类、离子液体用量、底物比例等因素的影响规律,结果表明,[BMIM]HSO 4用量为0.8 mmol,n(N-羟乙基苯胺)∶[KG-*3/5]n(丙烯腈)=1∶[KG-*3/5]1.2,反应温度为90℃,反应时间为12 h时,N-氰乙基-N-羟乙基苯胺产率最高(89%),离子液体循环使用5次后,催化活性基本保持不变。N-Cyanoethyl-N-hydroxyethylaniline is an important dye intermediate with a wide range of applications.A green and efficient protocol for the synthesis of N-cyanoethyl-N-hydroxyethylaniline by reaction of acrylonitrile and N-hydroxyethyl aniline with 1-butyl-3-methylimidazolium hydrosulphates ionic liquid([Bmim]HSO 4)as the catalyst has been developed,eliminating the inert-gas welding and complex operation of traditional methods.The effect of ionic liquid,the amount of ionic liquid,the ratio of substrates,temperature and time were investigated.The optimum reaction conditions were obtained as follow:[BMIM]HSO 40.8 mmol,n(N-hydroxyethyl aniline)∶[KG-*3/5]n(acrylonitrile)=1∶[KG-*3/5]1.2,reaction time of 12 h,reaction temperature of 90℃.The acdic ionic liquid could be easily separated and reused for at least 5 times without significantly decrease in catalytic activity.

关 键 词：酸性离子液体 N-氰乙基-N-羟乙基苯胺 丙烯腈 N-羟乙基苯胺 

分 类 号：O625.6[理学—有机化学]