用邻氰基氯苄的副产物合成盐酸肼屈嗪的研究  

SYNTHESIS OF HYDRALAZINE HYDROCHLORIDE WITH BY PRODUCTSIN MANUFACTURE OF o-CYANOBENZYLCHLORIDE

作　　者：李树安[1] 张珍明[1] 于亚丰 宋长生[1] 葛洪玉[1] 

机构地区：[1]淮海工学院化学工程学院,江苏连云港222005

出　　处：《精细石油化工》2008年第2期32-35,共4页Speciality Petrochemicals

基　　金：江苏省高校高新技术产业发展项目(JHB05-50);2006年江苏省教育厅"青蓝工程"学科带头人项目

摘　　要：用生产邻氰基氯苄的副产物[w(邻氰基甲苯)=10%、w(邻氰基氯苄)=30%和w(邻氰二氯苄)=50%]合成了盐酸肼屈嗪,探讨了反应温度、反应时间及投料比对邻氰基苯甲醛和盐酸肼屈嗪收率的影响。最佳合成条件:1)将邻氰基氯苄的副产物在引发剂作用下于150～155℃深度氯化,产物中邻氰二氯苄质量分数大于85%;2)n(邻氰二氯苄):n(甲醇钠)=1:2.05,回流反应20h,制得缩醛;3)n(缩醛):n(盐酸)=1:3.9,在0℃酸解反应3h,得到邻氰基苯甲醛,收率90.5%;4)n(邻氰基苯甲醛):n(85%的水合肼)=1:3.5,pH=3,回流时间8h,盐酸肼屈嗪收率75%。Hydralazine hydrochloride was synthesized from the by-products, containing o-cyanotoluene, o-cyanobenzylchloride and o-cyanobenzalchloride with the mass percentage of 10%, 30% and 50%, respectively, generated from the manufacture of o-cyanobenzylchloride. The effects of reaction temperature and time and ratios of raw materials on the yield of o-cyanobenzaldehyde and hydralazine hydrochloride were investigated. The procedures and optimal conditions were found as follows： Firstly, the by-product reacted with chlorine at 150 - 155 ℃, in the presence of initiator, to give o-cyanobenzalchloride with purity of above 85 %; Secondly, o-cyanobenzalchloride and sodium methoxide, in molar ratio of 1 ： 2.05, were refluxed for 20 h to produce the corresponding acetall Thirdly,the prepared acetal was hydrolyzed with HCl, in n（acetal） ： n（HCl） = 1 ： 3.9, at 0 ℃ for 3 h to obtain o- cyanobenzaldehyde with the yield of 90.5 %; Finally, hydralazine hydrochloride was synthesized with the yield of 75 % by refluxing o-cyanobenzaldehyde and hydrazine for 8 h at the molar ratio of 1 ： 3.5 in the presence of HCl and methanol.

关 键 词：肼屈嗪 邻氰基苯甲醛 邻氰基氯苄 副产物 

分 类 号：TQ463[化学工程—制药化工]