用Skraup反应合成7-氯喹哪啶  

Synthesis of 7-Chloroquinaldine by Skraup Reaction

作　　者：李树安[1] 张珍明[1] 张喆[1] 刘嵘森 葛洪玉[1] 

机构地区：[1]淮海工学院化学工程系,江苏连云港222005

出　　处：《淮海工学院学报（自然科学版）》2007年第3期49-51,共3页Journal of Huaihai Institute of Technology:Natural Sciences Edition

基　　金：江苏省高校高新技术产业发展项目(JHB05-50);江苏省教育厅"青蓝工程"资助项目

摘　　要：研究了以邻硝基甲苯为氧化剂,间氯苯胺和巴豆醛通过经典的Skraup反应制备7-氯喹哪啶的改进方法。7-氯喹哪啶的收率为46.7%,质量分数99.2%;副产物为二氯喹哪啶,收率13.4%。还考察了氧化剂、氧化剂的用量以及盐酸的浓度对7-氯喹哪啶收率的影响。在1 000 L反应釜上做了放大实验,共生产7 t 7-氯喹哪啶,质量和收率达到了小试的结果。Using o-nitrotoluene as an oxidant, the improved preparation of 7-chloroquinldine was studied by classical Skraup reaction of m-chloroaniline and crotonaldehyde. 7-chloroquinaldine was obtained with the yield rate of 46.7% and the purity of 99.2%. The side product was obtained and elucidated as dichloroquinaldine with the yield of 13.4%. The effect of oxidant, amount of oxidant and concentration of hydrochloric acid on the yield of 7-chloroquinaldine was also investigated. Scale-up of this procedure in the reactor of 1 000 L was carried out to yield 7 tons of 7- chloroquinaldine. The yield and quality of the product were the same as that of laboratory-scale.

关 键 词：7-氯喹哪啶 间氯苯胺 巴豆醛 邻硝基甲苯Skraup合成 中试放大 

分 类 号：O621.25[理学—有机化学]