第 45 卷第 2 期Vol. 45 No. 2
2015 年 4 月Apr 2015

所属栏目:农药及中间体

2,5-二甲基苯乙酸合成工艺改进研究
邹建平1,2,3,尹笃林1,赵东江2,3,5,陈蒙慈4,杨 彬2,3,5,陈 明2,3* (1. 湖南师范大学 化学化工学院,湖南 长沙 410081;2. 湖南化工研究院 国家农药创制工程技术研究中心,湖南 长沙 410014;3. 农用化学品湖南省重点实验室,湖南 长沙 410014;4. 湖南海利化工股份有限公司,湖南 长沙 410007;5. 湖南大学 化学化工学院,湖南 长沙 410082)
摘 要:以对二甲苯为原料,经氯甲基化、氰化和酸性水解制备2,5-二甲基苯乙酸。通过优化氯甲基化反应的条件,大幅度降低了二取代产物的量;通过氰基酸性水解避免了碱性水解法产品难过滤、含盐废水大的问题。总收率77.9%,含量99%以上。
关键词:2,5-二甲基苯乙酸;氯甲基化;氰化;酸性水解
中图分类号:S482.5+2  文献标识码:A  文章编号:1009-9212(2015)02-0020-03
Improvement on Synthetic Method of 2,5-Dimethylphenylacetic Acid
ZOU Jian-ping1,2,3, YIN Du-lin1, ZHAO Dong-jiang2,3,5, CHEN Meng-ci4, YANG Bing2,3,5, CHEN Ming2,3* (1. School of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, China; 2.Hunan Research Institute of Chemical Industry, National Engineering Research Centre for Agrochemicals, Changsha 410014, China; 3. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 4. Hunan Haili Chemical Industry Co., Ltd., Changsha 410007, China; 5. School of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, China)
Abstract:2,5-Dimethylphenylacetic acid was obtianed through a series of reactions including chloromethylation, cyanidation, and acid hydrolysis using para-xylene as the starting material. The content of two substituted impurities was greatly reduced through optimizing the reaction conditions for chloromethylation. The work-up process was greatly improved by the changing the hydrolysis condition from basic to acidic. In this process, the filtration of a large quantity of salinity wastewater was avoided. A total yield of 77.9% with purity over 99% was obtained.
Key words:2,5-dimethylphenylacetic acid; chloromethylation; cyanidation; acid hydrolysis
作者简介:邹建平(1990-),男,湖南郴州人,硕士研究生,主要从事农药合成工艺研究(E-mail:zou2998@163.com)。
联 系 人:陈 明,研究员,主要从事农药及其中间体合成工艺研究(E-mail:chegming1@163.com)。
收稿日期:2015-01-19