摘要
在氢氧化钾参与下,利用固-液相转移催化法合成了标题化合物,实验考察了不同催化剂、催化剂用量、反应物用量、反应温度对收率的影响,结果表明:以聚乙二醇-400为催化剂,且其物质的量为底物2-苯基-4-氯甲基硒唑的5%,2-苯基-4-硒唑基氯甲烷和2-氨基-5-巯基-1,3,4-噻二唑的物质的量比为1∶1.2,在丙酮中回流,为较佳反应条件,收率可达82.6%,目标物的结构经IR、1HNMR及ESI-MS等方法确证。
2-Amino-5 - （ 2-phenyl-1,3 -se｜enazol-4-methylthio ） - 1,3,4-thiadiazole was synthesized by the reaction of 2-phen- y]-4-chloromethylselenazole and 2-amino-5-mercapto-1,3,4- thiadiazole under the conditions of solid-liquid phase transfer catalysts in the presence of potassium hydroxide with acetone as the solvent. The effects of different phase transfer catalyst, amount of eata｜yst and reactants, temperature on the yield were discussed. The optimum reaction conditions were ob- tained as follows ： the molar ratio of ：2-phenyl-4-chloromethyl- selenazole and 2-amino-5-mercapto-1, 3, 4-thiadiazole is 1： 1.2,the molar amount of the catalyst to 2-phenyl-4-chlo- romethylselenazole is 5% ,PEG-400 is a phase transfer under reflux. The structure of product was confirmed by IR,1HNMR and ESI-MS,the total yield was 82.6%.
出处
《化学试剂》
CAS
CSCD
北大核心
2013年第3期206-208,共3页
Chemical Reagents
基金
国家自然科学基金资助项目(20971097)
