摘要
以乙醇胺为起始原料,经三甲基氯硅烷保护制得2-(三甲基硅氧基)乙胺,再经与二硫化碳反应,再与溴乙烷缩合得到N-(2-三甲基硅氧乙基)二硫代氨基甲酸乙酯、然后再与叠氮化钠成环反应合成了1-(2-三甲基硅氧乙基)-5-巯基四氮唑。用三甲基氯硅烷作为乙醇胺的羟基保护试剂,保护和脱保护具有反应条件温和、收率高等优点,反应总收率高达85%以上。
1-(2-hydroxyethyl)-1H-tetrazole-5-thiol was synthesized from ethanolamine as the starting material,via hydroxyl protection with trimethyl chlorosilane,react with carbon bisulfide? then condensation with bromoethane get 1-(2-trimethylsilanyloxy-ethyl)dithiocarbamic acid ethyl ester;it cyclization with sodium azide get 1-(2-trimethylsilanyloxy-ethyl)-1H-tetrazole-5-thiol.The protection and deprotection processes have advantages of mild reactive condition,high yield,the overall yield was over 85%.
出处
《化工时刊》
CAS
2011年第5期25-26,37,共3页
Chemical Industry Times