氨噻肟酸的合成  

Synthesis of 2-(2-Aminothiazole-4-yl)-2-(Z)-methoxyiminoacetic Acid

作　　者：徐娟娟[1] 胡艾希[1] 

机构地区：[1]湖南大学化学化工学院,湖南长沙410082

出　　处：《精细化工》2007年第4期385-386,396,共3页Fine Chemicals

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。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.

关 键 词：氨噻肟酸 4-氯乙酰乙酸乙酯 肟化反应 

分 类 号：O626.25[理学—有机化学]