3-乙氧基-4-甲氧基苯腈的合成  

SYNTHESIS OF 3-ETHOXY-4-METHOXYBENZONITRILE

作　　者：张思科 岳金方[2] 王雪源[2] 静巍 罗志臣 刘伟[2] 陈柯全[2] Zhang Sike;Yue Jinfang;Wang Xueyuan;Jing Wei;Luo Zhichen;Liu Wei;Chen Kequan(College of Chemistry and Pharmaceutical Engineering,J ilin Institute of Chemical Technology,Jilin 132022,Jilin,China;College of Chemical Engineering,Yangzhou Polytechnic Institute,Yangzhou 225127,Jiangsu,China)

机构地区：[1]吉林化工学院化学与制药工程学院,吉林吉林132022 [2]扬州工业职业技术学院化学工程学院,江苏扬州225127

出　　处：《精细石油化工》2018年第5期21-24,共4页Speciality Petrochemicals

基　　金：江苏省高等学校自然科学研究面上项目资助项目(17KJB150046);江苏省高等学校优秀科技创新团队(苏教科[2017]6号);扬州工业职业技术学院专业导师工作室(2016-01);科研创新团队(2016-001)资助课题

摘　　要：以异香兰素为原料,经O-烷基化反应和氰基化反应制备医药中间体3-乙氧基-4-甲氧基苯腈,考察了O-烷基化反应和氰化反应的影响因素。实验表明:制备3-乙氧基-4-甲氧基苯甲醛的最佳合成工艺条件为:异香兰素45.6g(0.30mol),n(异香兰素)∶n(溴乙烷)=1∶1.15,0.5 MPa于85℃反应5h,3-乙氧基-4-甲氧基苯甲醛的收率达到97%以上;以3-乙氧基-4-甲氧基苯甲醛为原料,经氰化反应制备3-乙氧基-4-甲氧基苯腈的最佳工艺条件为:在乙酸介质中,3-乙氧基-4-甲氧基苯甲醛与盐酸羟胺的摩尔比为1.0∶1.5,于70~80℃下反应4h,3-乙氧基-4-甲氧基苯腈的收率超过91%,纯度99.4%。The methods for preparing 3-ethoxyl-4-methoxybenzene nitrile have been studied by o-alkylation reaction and cyanidation of isovanillin.The effects on O-alkylation reaction and cyanidation reaction were investigated.Experiments show that the optimum synthetic process conditions for preparation of 3-ethoxy-4-methoxy benzaldehyde：isovanillin 45.6 g（0.30 mol）,isovanillin and bromine ethane mole ratio was 1∶1.15,after 5 h,the yield of 3-ethoxy-4-methoxy benzaldehyde reached above 97%at 0.5 MPa and 85℃;3-ethoxy-4-methoxy benzaldehyde as raw material,optimum technological conditions for preparation of 3-ethoxyl-4-methoxybenzene nitrile by cyanide reaction were：in acetic acid medium,3-ethoxy-4-methoxy benzene,formaldehyde and hydroxylamine hydrochloride mole ratio 1.0∶1.5,after 4 h,3-ethoxyl-4-methoxybenzene nitrile yield more than 91%,the purity of 99.4% at 70-80 ℃.This method has following advantages：mild reaction conditions,cheap raw materials,high yield,good purity and suitable for industrial production.

关 键 词：异香兰素 3-乙氧基-4-甲氧基苯腈 O-烷基化 氰化 

分 类 号：TQ246.7[化学工程—有机化工]