摘要
以苦参碱为原料,通过碱水解开环,溴乙烷乙基化得到N-乙基苦参酸乙酯,继而水解得到N-乙基苦参酸,最后在脱水剂作用下与百里酚缩合,得到N-乙基苦参酸百里酚酯。目标化合物的化学结构经红外光谱、核磁共振氢谱及质谱确证。考察了N-乙基苦参酸与百里酚缩合反应中脱水剂、反应物配比、温度等因素对产率及反应时间的影响,优选出最佳合成工艺。最佳合成工艺为:以1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐(EDCI)为脱水剂,反应物配比为n(N-乙基苦参酸)∶n(百里酚)=1∶1.5,反应温度45~50℃,该条件下N-乙基苦参酸百里酚酯的收率达60.6%。
Matrine was reacted with sodium hydroxide to give the hydrolytic ring-opening derivative matrinic acid,which was condensed with bromoethane to yield N-ethyl matrinate.The matrinate was hydrolyzed to give N-ethyl matrinic acid,which was coupled with thymol in the presence of EDCI to provide the target compound.Its chemical structure was confirmed by IR,MS,and 1 H NMR spectroscopy.The effect of the ratio of N-ethyl matrinic acid to thymol and the reaction temperature on the yield of the target compound was studied.The optimum reaction conditions were as follows:N-ethyl matrinic acid:thymol=1∶1.5(n∶n),and reaction temperature at 45~50℃.The yield of thymol N-ethyl matrinate was 60.6%.
出处
《化学世界》
CAS
CSCD
北大核心
2014年第5期289-291,296,共4页
Chemical World
基金
安徽省教育厅自然科学重点科研项目(KJ2013A168)