2-氨基-1-甲基-1H-咪唑-5-羧酸乙酯的合成  

Synthesis of 2-amino-1-methyl-1H-imidazol-5-carboxylic acid ethyl ester

作　　者：林联君 杨艳萍 董林娟 LIN Lian-jun;YANG Yan-ping;DONG Lin-juan(Faculty of Health,Shaanxi Fashion Engineering University,Xi'an 712046,China)

机构地区：[1]陕西服装工程学院,陕西西安712046

出　　处：《化学工程师》2023年第9期11-13,18,共4页Chemical Engineer

基　　金：2022年度陕西服装工程学院校级教学改革研究项目(2022J003);2021年度陕西服装工程学院大学生创新创业训练计划项目(S202113125024)。

摘　　要：以肌氨酸乙酯盐酸盐为起始原料,经氨酯交换反应、Claisen-Schmidt反应、合环反应共3步反应,得到目标产物2-氨基-1-甲基-1H-咪唑-5-羧酸乙酯(1),产物结构经^(1)H NMR确证。优化了反应条件:第一步,n_((肌氨酸乙酯盐酸盐))∶n_((K2)CO_(3))=1∶1.5,反应时间为8h,反应温度为25℃;第二步,n_((3))∶n_((NaH))=1∶1.2;第三步,n_((4))∶n_((NH2)CN)=1∶2.5,n_((4))∶n_((NaOAc))=1∶3.2,优化条件下的总收率为43.7%。此合成途径操作简便、产品质量好、总收率高,利于大量生产。The target product 2-amino-1-methyl-1H-imidazol-5-carboxylic acid ethyl ester(1)was obtained from the sarcosine ethyl ester hydrochloride as the starting material through three steps of transesterification,Claisen-Schmidt reaction and cyclization reaction.The structure of the product was confirmed by ^(1)H NMR.The reaction conditions were optimized:in the first step,n_((Sarcosine ethyl ester hydrochloride))∶n_((K_2CO_3))=1∶1.5,reaction time 8h,reaction temperature 25℃;In the second step,n_((3))∶n_((NaH))=1∶1.2;In the third step,n_((4))∶n_((NH_2CN))=1∶2.5,n(3)∶n(NaOAc)=1∶3.2,the total yield under the optimum conditions was 43.7%.This synthetic route is easy to operate,with good product quality and high total yield,which is more conducive to mass production.

关 键 词：2-氨基-1-甲基-1H-咪唑-5-羧酸乙酯 Claisen-Schmidt反应 合成 优化 

分 类 号：TQ463[化学工程—制药化工]