AE-活性酯的合成  

Synthesis of AE-active Ester

作　　者：葛洪玉[1] 马卫兴[1] 许兴友[1] 

机构地区：[1]淮海工学院化学工程系,江苏连云港222005

出　　处：《江苏化工》2007年第1期32-34,共3页Jiangsu Chemical Industry

基　　金：江苏省高校高新技术产业发展项目(JHB05-50);江苏省高校自然科学研究计划资助项目(05KJB15003);淮海工学院自然科学研究基金资助项目(Z2004026)

摘　　要：研究了AE-活性酯的合成工艺。以乙酰乙酸乙酯为原料,以乙醇和四氢呋喃的混合溶液做溶剂,亚硝酸乙酯作为肟化剂,采用连续投料方式,一个单元操作内完成溴化、肟化、环合和甲基化反应制得氨噻肟酸乙酯,在NaOH的乙醇水溶液中于50℃水解后再与促进剂DM缩合得到目标化合物AE-活性酯,总收率为52.3%,质量分数为98.8%。合成工艺不仅缩短了反应时间,将总收率提高12%,同时提高了溶济回收率,减少了环境污染。The synthetic technique of AE-active ester is studied in this paper. Ethy-aminothiazolyloximate(3)was prepared by bromination oximation,cyclization and methylation from ethyl-acetoacetate within a steps sequential to give the yields of 73.8%,for which the ethyl nitrite was used as the oximation agent in the component solvent of ethanol and teteahydrofunan. The obtained product was further hydrolysis with NaOH solution at 50 ℃ to give(Z)-2-(2-aminothiazole-4-yl)-2-methoxyiminoacetic acid(4). For preparation of the title product(1),the condensation reaction of the compound(4)with the accelerating agent DM was performed by using 1,2-dichloroethane as solvent with the overall yield 52.3% and mass fraction of 98.8%. this process not only shortened reaction time,but also increased the yield for 10% and the recycle percent of solvent.

关 键 词：AE-活性酯 氨噻肟酸乙酯 乙酰乙酸乙酯 合成 

分 类 号：TQ252.5[化学工程—有机化工]