| 氨噻肟酸的合成 |
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| 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 |
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| 作者姓名： | 徐娟娟 胡艾希 |
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| 作者单位： | 湖南大学,化学化工学院,湖南,长沙,410082;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 |
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| 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。
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| 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 |
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| 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 |
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| Authors: | XU Juan-juan HU Ai-xi |
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| 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 |
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| 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. |
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| Keywords: | 2-(2-aminothiazole-4-yl)-2-(Z)-methoxyiminoacetic acid ethyl 4-chloroacetoacetate oximation |
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