除草剂特丁噻草隆的合成工艺优化  

Synthesis process optimization on herbicide tebuthiuron

作　　者：王磊[1] WANG Lei(Department of Food and Environmental Engineering,Chuzhou Vocational and Technical College,Chuzhou,239000,China)

机构地区：[1]滁州职业技术学院食品与环境工程系

出　　处：《佛山科学技术学院学报（自然科学版）》2019年第3期48-51,共4页Journal of Foshan University(Natural Science Edition)

基　　金：安徽省高校自然科学研究项目(KJ2018A0840);安徽省高校优秀青年人才支持计划重点项目(gxyqZD2017123)

摘　　要：以2-甲胺基-5-特丁基-1,3,4-噻二唑(MTBA)与固体光气(BTC)、甲胺反应得到除草剂特丁噻草隆,产物结构经UV、IR和1HNMR表征。经单因素实验,确定了合成特丁噻草隆的最优条件:以甲苯为溶剂,nMTBA:nBTC=1:0.43,于80℃滴加BTC,回流反应3h,然后在10℃下加入甲胺,110℃反应3h,得到产物,收率75.3%。该工艺采用BTC代替剧毒品光气,减少了副产物的生成,提高了收率和生产的安全性,适于工业化生产。Tebuthiuron was synthesized by reaction of 2-methylamino-5-tert-butyl-1,3,4-thiadiazole (MTBA)with triphosgene (BTC) and methylamine. The structures of product were characterized by UV、IR and 1HNMR.The optimum reaction conditions for synthesis of tebuthiuron were as follows: The yield of Tebuthiuron was 75.3% under the optimum conditions with the ratio of n(MTBA):n(BTC)=1:0.43, BTC added at 80℃,refluxing for 3hs in toluene, then methylamine dropped at the temperature below 10℃, added at 110℃ for another 3hs.The process uses BTC instead of the drug phosgene, which reduces the formation of by-products, improves the yield and production safety, and is suitable for industrial production.

关 键 词：除草剂 2-甲胺基-5-特丁基-1 3 4-噻二唑 特丁噻草隆 固体光气 甲胺 

分 类 号：TQ457.2[化学工程—农药化工]