摘要
以二苯乙腈和二溴乙烷为原料,苯扎溴铵为相转移催化剂,在氢氧化钠水溶液中高效合成溴乙基二苯乙腈。分别考察了不同相转移催化剂、碱的种类及用量、原料配比对反应收率和选择性的影响,优化反应条件,得到了溴乙基二苯乙腈的最佳合成工艺,同时实现了两种相关杂质的定向合成。溴乙基二苯乙腈2及两种相关杂质3和4的结构经^(1)H NMR,^(13)C NMR和MS(EI)确证。
Bromoethyl diphenylacetonitrile was efficient synthesized from diphenylacetonitrile and dibromoethane in sodium hydroxide aqueous solution by phase transfer catalyst of benzalkonium bromide.Effects of different phase transfer catalyst,base,base dosage and raw material ratio on the yield and selectivity of the reaction were investigated.After optimized the reaction conditions,the best synthesis technology of bromoethyl diphenylacetonitrile and the ific synthesis of two impurities have been achieved.The structures of bromoethyl diphenylacetonitrile 2 and the two impurities of 3 and 4 were characterized by ^(1)H NMR,^(13)C NMR and MS(EI),respectively.
作者
袁伟
殷晓伟
杨科
李正义
YUAN Wei;YIN Xiaowei;YANG Ke;LI Zhengyi(Jiangsu Key Laboratory of Advanced Catalytic Materials and Technology, School of Petrochemical Engineering, Changzhou University, Changzhou 213164, China;Changzhou Kangpu Pharmaceutical Co., Ltd., Changzhou 213172, China)
出处
《合成化学》
CAS
2022年第7期569-573,共5页
Chinese Journal of Synthetic Chemistry
基金
江苏省先进催化与绿色制造协同创新中心资助项目(ACGM2019-05-08)。
关键词
溴乙基二苯乙腈
合成
杂质
相转移催化
医药中间体
bromoethyl diphenylacetonitrile
synthesis
impurity
phase transfer catalysis
pharmaceutical intermediates
作者简介
第一作者:袁伟(1997-),男,汉族,江苏泰州人,硕士,主要从事药物合成及质量控制研究,E-mail:1418682112@qq.com;通信联系人:李正义,博士,教授,硕士生导师,E-mail:zyli@cczu.edu.cn。
