4-甲基苯腈合成研究  

Research on the synthesis of 4-methylbenzonitrile

作　　者：王恰如 王艳娇[1] 朱周静 唐文强 WANG Qia-ru;WANG Yan-jiao;ZHU Zhou-jing;TANG Wen-qiang(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China;Xianyang Key Laboratory of Molecular Imaging and Drug Synthesis,Xianyang 712046,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西咸阳712046 [2]咸阳市分子影像与药物合成重点实验室,陕西咸阳712046

出　　处：《精细与专用化学品》2024年第10期39-41,共3页Fine and Specialty Chemicals

基　　金：陕西省大学生创新创业训练计划项目(S202313123046);陕西国际商贸学院“中药药效物质研究”创新团队资助项目(SSY18TD01);咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008)。

摘　　要：以1,4-二溴苯为原料,依次经历氰基取代和Suzuki偶联反应得到产物4-甲基苯腈,其结构经1HNMR和ESI-MS表征。分别对两步反应条件进行优化,确定氰化反应的适宜条件为:物料比n(氰化亚铜)∶n(1,4-二溴苯)=1.1∶1、反应温度为110℃、反应时间为16h。在该条件下,4-溴苯腈的收率达到67.5%(以1,4-二溴苯计)。Suzuki偶联反应的适宜条件为:反应溶剂为N,N-二甲基甲酰胺、催化剂为Pd(PPh3)4,4-甲基苯腈收率达到81.2%(以4-溴苯腈计)。The product 4-methylbenzonitrile was prepared from 1,4-dibromobenzene via cyanide substitution and Suzuki coupling reaction.The structure of the product was characterized by ~1HNMR and ESI-MS.The two-step reaction conditions were optimized respectively.The optimum conditions for cyanidation were as follows: material ratio n(CuCN)∶n(1,4-dibromobenzene)=1.1∶1,at temperature of 110℃ for 16h, the yield of 4-bromobenzonitrile was up to 67.5%(calculated as 1,4-dibromobenzene).The optimum conditions of Suzuki coupling reaction were as follows: the reaction solvent was DMF,the catalyst was Pd(PPh_3)_4,and the yield of 4-methylbenzonitrile was 81.2%(calculated as 4-bromobenzonitrile).

关 键 词：4-甲基苯腈 芳香腈化合物 氰化反应 SUZUKI偶联反应 条件优化 

分 类 号：TQ463[化学工程—制药化工]