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。
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 by1HNMR 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.
出处
《日用化学工业》
CAS
CSCD
北大核心
2014年第1期15-18,共4页
China Surfactant Detergent & Cosmetics
基金
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)
关键词
季鏻盐
三苯基膦
卤代烃
微波辐射
quaternary phosphonium salt
triphenylphosphine
halogenated hydrocarbon
microwave irradiation
