药用中间体1-甲基-5-巯基-1H-四氮唑相转移合成工艺研究  

Synthesis of 5-mercapto-1-methyltetrazole by phase transfer catalysis

作　　者：常相娜[1] 张健宇 宁肖肖 沈文[1] 

机构地区：[1]陕西科技大学生命科学与工程学院,陕西西安710021 [2]杨凌示范区食品药品检验所,陕西杨凌712100

出　　处：《陕西科技大学学报（自然科学版）》2015年第1期131-135,共5页Journal of Shaanxi University of Science & Technology

基　　金：陕西省科技厅自然科学基础研究计划项目(2011JM2005);陕西省教育厅专项科研计划项目(2013JK0767)

摘　　要：在水相中,相转移催化剂催化条件下合成1-甲基-5-巯基-1H-四氮唑,并对其工艺条件进行研究.采用IR与1 HNMR对产物结构进行了表征.结果表明催化剂的最优制备条件为:催化剂为环糊精、蒸馏水加入量为30mL、催化剂加入量为1%(占叠氮钠的摩尔百分数).在此催化条件下优化工艺条件为:异硫氰酸甲酯与叠氮钠的摩尔比为1.4∶1.0;滴加完异硫氰酸甲酯后的反应时间为2h;反应温度为75℃.产物收率为76.93%.In the presence of phase-transfer catalyst,5-mercapto-1-methyltetrazole was synthesized in aqueous phase.The structure was characterized by means of IR and 1 H NMR.The optimum condition of phase transfer catalyst were ascertained as follows：the phase transfer catalyst was cyclodextrin,the quality of deionized water was 30 mL,and the quality ratio of phase transfer catalyst and sodium azide was 1∶100（mol/mol）.Using cyclodextrin as phase transfer catalyst,the optimum preparation procedure was：reaction temperature was 70 ℃,the quality ratio of methyl isothiocyanate and sodium azide was 1.4∶1.0（mol/mol）,reaction time was 2h,and the yield of 5-mercapto-1-methyltetrazole was 79.63%.

关 键 词：1-甲基-5-巯基-1H-四氮唑 相转移催化 工艺 

分 类 号：R97[医药卫生—药品]