摘要
报道了一种合成重要的医药中间体2-巯基-5-甲基-1,3,4-三氮唑的新方法。第一步,以乙酸代替吡啶/乙酰氯体系,和氨基硫脲发生酰化反应,得到N-乙酰基氨基硫脲,反应时间从24h缩短至5h;第二步,在微波辐射下,用1mol/L NaOH水溶液代替甲醇钠/甲醇溶液,中间体N-乙酰基氨基硫脲环合为2-巯基-5-甲基-1,3,4-三氮唑。该法反应时间短,原料廉价易得,中间体和产物的分离纯化不需要柱层析,为规模生产提供了条件。
The new method for synthesis of 2-mercapto-5-methyl-1,3,4-triazole was presented. Thio- semicarbazide was acetylated by acetic acid instead of pyridine/acetlyl chloride to afford acetyhhiosem- icarbazide. The reaction time reduced to 5 hours from 24 hours. Under microwave irradiation, acetyl- thiosemicarbazide was cyclizated into 2-mercapto-5-methyl-1,3,4-triazole in 1 mol/L NaOH instead of reported CH30Na/CH3 OH. The reaction rate was increased by 80 times. This method takes advanta- ges of short reaction time, available raw materials and easy purification with the promise for scale ex- pansion.
出处
《精细石油化工》
CAS
CSCD
北大核心
2013年第2期37-39,共3页
Speciality Petrochemicals
关键词
1
3
4-三氮唑
氨基硫脲
微波
酰化
1,3,4-triazole
thiosemicarbazide
microwave irradiation
acetylation
