微波辅助法合成季鏻盐

doi:10.13218/j.cnki.csdc.2014.01.004

日用化学工业 ›› 2014, Vol. 44 ›› Issue (1): 15-18.doi: 10.13218/j.cnki.csdc.2014.01.004

微波辅助法合成季鏻盐

尹晓刚^1,2, 赵正容¹, 肖维军¹, 陈卓¹, 于杰²

1.贵州师范大学化学与材料科学学院贵州省功能材料化学重点实验室,贵州贵阳 550001;
2.国家复合改性聚合物材料工程技术研究中心,贵州贵阳 550014

收稿日期:2013-08-26 发布日期:2019-04-09
通讯作者: 陈卓,教授,电话:(0851)6700050,E-mail:chenzhuo19@163.com。
作者简介:尹晓刚(1976-),男,江苏人,副教授,博士,电话:(0851)6700050。
基金资助:
国家自然科学基金资助项目(No.20862004);973计划前期研究专项资助项目(2011CB612313);2012贵州师范大学国家级大学生创新创业训练计划资助项目(201210663005)

Synthesis of quaternary phosphonium salts under assistance of microwave irradiation

YIN Xiao-gang^1,2, ZHAO Zheng-rong¹, XIAO Wei-jun¹, CHEN Zhuo¹, YU Jie²

1.Key Laboratory of Functional Materials Chemistry of Guizhou Province,School of Chemistry and Materials Science, Guizhou Normal University,Guiyang,Guizhou 550001,China;
2.National Engineering Research Center for Compounding and Modification of Polymeric Materials,Guiyang,Guizhou 550014,China

Received:2013-08-26 Published:2019-04-09

摘要/Abstract

摘要： 以三苯基膦和卤代烃为原料,采用微波法合成了7种季鏻盐。考察了反应温度、反应时间、溶剂种类、溶剂用量及原料摩尔比对产物产率的影响,确定了微波辅助法合成季鏻盐的较优条件:以DMF,乙腈或甲苯为溶剂、反应时间为20 min、反应温度为120 ℃、三苯基膦与卤代烃的摩尔比为1.1∶1、三苯基膦在反应体系中的浓度为2.86 mol·L^-1。在此条件下,苄基三苯基溴化鏻产率可达93.5%,其他季鏻盐产率也较为理想。使用熔点仪和核磁共振波谱仪对合成的季鏻盐进行了表征。在较优条件下,微波法合成季鏻盐所需时间仅为传统加热法的2.8%以下。

关键词: 季鏻盐, 三苯基膦, 卤代烃, 微波辐射

Abstract: Seven kinds of quaternary phosphonium salt were synthesized with halogenated hydrocarbons and triphenylphosphine as starting materials under assistance of microwave irradiation.Effects of reaction temperature,time,kind of solvent,solvent dosage and the molar ratio were studied,and the optimal conditions of the reaction were determined as:adopting DMF,acetonitrile or toluene as the solvent;reaction time,20 min;reaction temperature,120 ℃;molar ratio of triphenylphosphine and halogenated hydrocarbon,1.1∶1;concentration (measured by moles of triphenylphosphine),2.86 mol·L^-1.Under the above mentioned conditions,yield of benzyltriphenylphosphonium bromide product can achieve 93.5%;while yield of other kinds of the quaternary phosphonium salt are also satisfactory.The products were characterized by ¹HNMR and melting point.Under optimal conditions,the time needed for completion of the reaction is no more than 2.8% of that of conventional heating methods.

Key words: quaternary phosphonium salt, triphenylphosphine, halogenated hydrocarbon, microwave irradiation

中图分类号:

TQ423.12

尹晓刚, 赵正容, 肖维军, 陈卓, 于杰. 微波辅助法合成季鏻盐[J]. 日用化学工业, 2014, 44(1): 15-18.

YIN Xiao-gang, ZHAO Zheng-rong, XIAO Wei-jun, CHEN Zhuo, YU Jie. Synthesis of quaternary phosphonium salts under assistance of microwave irradiation[J]. China Surfactant Detergent & Cosmetics, 2014, 44(1): 15-18.

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微波辅助法合成季鏻盐

Synthesis of quaternary phosphonium salts under assistance of microwave irradiation

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