Hu Ai-xi
2007
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Journal
Fine chemicals
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.