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氨噻肟酸的合成
引用本文:徐娟娟,胡艾希.氨噻肟酸的合成[J].精细化工,2007,24(4):385-386,396.
作者姓名:徐娟娟  胡艾希
作者单位:1. 湖南大学,化学化工学院,湖南,长沙,410082
2. 湖南大学,化学化工学院,湖南,长沙,410082;华南理工大学,化工与能源学院,广东,广州,510640
摘    要:4-氯乙酰乙酸乙酯经亚硝酸异丙酯肟化、硫脲环合一步反应制得去甲氨噻肟酸乙酯。反应条件为:n(4-氯乙酰乙酸乙酯)∶n(亚硝酸异丙酯)=1∶1.05,肟化反应温度为10~12℃,肟化反应、环合反应时间分别为22、3.5h。去甲氨噻肟酸乙酯经甲基化、水解反应后得到氨噻肟酸,总收率46.3%(以4-氯乙酰乙酸乙酯计)。产物经1HMNR表征,符合结构特征。

关 键 词:氨噻肟酸  4-氯乙酰乙酸乙酯  肟化反应
文章编号:1003-5214(2007)04-0385-03
修稿时间:2006-10-142006-11-13

Synthesis of 2-(2-Aminothiazole-4-yl)-2-(Z)-methoxyiminoacetic Acid
XU Juan-juan,HU Ai-xi.Synthesis of 2-(2-Aminothiazole-4-yl)-2-(Z)-methoxyiminoacetic Acid[J].Fine Chemicals,2007,24(4):385-386,396.
Authors:XU Juan-juan  HU Ai-xi
Affiliation:1. College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, Hunan, China;2. School of Chemical and Energy Engineering, South China University of Technology, Guangzhou 510640, Guangdong, China
Abstract:Ethyl 4-chloroacetoacetate was oximated with isopropyl nitrite and then condensated with thiourea to give ethyl 2-(2-aminothiazole-4yl)-2-hydroxyiminoacetic acid.Mole ratio of ethyl 4-chloroacetoacetate and isopropyl nitrite was 1∶1.05,reaction temperature of oximation was 10~12 ℃,and reaction time of oximation and condensation were 22 h and 3.5 h,respectively.The ester was converted into 2-(2-aminothiazole-4-yl)-2-(Z)-methoxyiminoacetic acid via methylation and hydrolyzation.The total yield was 46.3 %(based on ethyl 4-chloroacetoacetate).Structures of the products were confirmed by 1HNMR.
Keywords:2-(2-aminothiazole-4-yl)-2-(Z)-methoxyiminoacetic acid  ethyl 4-chloroacetoacetate  oximation
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