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氧氯化法制备5-氯-8-羟基喹啉的研究
引用本文:张珍明,王丽萍,李树安,葛洪玉. 氧氯化法制备5-氯-8-羟基喹啉的研究[J]. 化工时刊, 2010, 24(5): 27-29. DOI: 10.3969/j.issn.1002-154X.2010.05.008
作者姓名:张珍明  王丽萍  李树安  葛洪玉
作者单位:1. 中国矿业大学环境与测绘学院,江苏,徐州,221116;淮海工学院,化学工程学院,江苏,连云港,222005
2. 中国矿业大学环境与测绘学院,江苏,徐州,221116
3. 淮海工学院,化学工程学院,江苏,连云港,222005
基金项目:江苏省海洋资源开发研究院基金,江苏省教育厅"青蓝工程"优秀学科带头人项目,江苏省连云港市科技局项目,淮海工学院绿色精品课程建设项目 
摘    要:研究了8-羟基喹啉、过氧化氢为主要原料通过氧氯化方法制备医药和农药的重要中间体5-氯-8-羟基喹啉的工艺条件。8-羟基喹啉、过氧化氢和30%盐酸投料比为1∶1.05∶16.7,在10~15℃下把过氧化氢滴加到8-羟基喹啉和盐酸的混和物中反应2 h,抽滤分离出5-氯-8-羟基喹啉盐酸盐,用盐酸萃取,用28%氨水中和至pH6.7得到5-氯-8-羟基喹啉,质量分数大于99%,收率为82.4%。研究了投料比、反应温度和时间对5-氯-8-羟基喹啉收率的影响。

关 键 词:5-氯-8-羟基喹啉  8-羟基喹啉  氧氯化反应  过氧化氢

Study on the Preparation of 5-chloro-8-hydroxyquinoline with Oxidative Chlorination
Zhang Zhenming,Wang Liping,Li Shuan,Ge Hongyu. Study on the Preparation of 5-chloro-8-hydroxyquinoline with Oxidative Chlorination[J]. Chemical Industry Times, 2010, 24(5): 27-29. DOI: 10.3969/j.issn.1002-154X.2010.05.008
Authors:Zhang Zhenming  Wang Liping  Li Shuan  Ge Hongyu
Affiliation:1.College of Environment and Surveying,China Mining University,Jiangsu Suzhou 221116;2.Dept.of Chemical Engineering,Huaihai Institute of Technology,Jiangsu Lianyungang 222005)
Abstract:5-chloro-8-hydroxyquinoline,an important intermediate used for medicine and agriculture,was prepared by oxidative chlorination of 8-hydroxyquinoline with H2O2.The optimam conditions were as follows: molar ratio of 8-hydroxyquinoline:H2O2∶30%HCl=1∶5∶1.1,and H2O2 added dropwise to the mixture of 8-hydroxyquinoline and hydrochloric acid at 10~15℃ for 4 h.After working up,5-chloro-8-hydroxyquinoline was obtained in 82.1% yield and 98.7% purity.The effects of ratio of raw materials,reaction temperature and time on the yield of 5-chloro-8-hydroxyquinoline were also investigated.
Keywords:5-chloro-8-hydroxyquinoline 8-hydroxyquinoline oxidative chlorination hydrogen peroxide
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