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以乙酰乙酰苯胺和二氯化砜为原料,通过氯代反应生成α-氯代乙酰乙酰苯胺。以水为溶剂,在酸催化下α-氯代乙酰乙酰苯胺与硫脲发生缩合反应制得2-氨基-4-甲基-5-苯甲酰胺噻唑,缩合反应的较优合成工艺条件:α-氯代乙酰乙酰苯胺与硫脲的质量比为1∶1.2、反应温度90℃、反应时间3h、浓盐酸0.5mL、H_2O 35mL。实验表明,α-氯代乙酰乙酰苯胺收率达到91.4%,2-氨基-4-甲基-5-苯甲酰胺噻唑收率达到94.7%,总收率达到87%。经红外、高液相色谱、~1H NMR表征证明合成产物为目标化合物。该合成技术工艺过程简单、生产安全、反应条件温和、生产成本降低、环境友好、产品收率高。
Acetoacetanilide and dimethylsulfoxide are used as raw materials to produce α-chloroacetoacetanilide by chlorination. Aqueous 2-amino-4-methyl-5-benzamidothiazole was synthesized from α-chloroacetoacetanilide and thiourea by acid catalysis under the catalysis of acid. The optimal synthesis conditions of α - chloroacetoacetanilide and thiourea mass ratio of 1: 1.2, the reaction temperature is 90 ℃, the reaction time 3h, concentrated hydrochloric acid 0.5mL, H_2O 35mL. The results showed that the yield of α-chloroacetoacetanilide reached 91.4%, the yield of 2-amino-4-methyl-5-benzamidothiazole reached 94.7% and the total yield reached 87%. Infrared and high liquid chromatography, ~ 1H NMR characterization of the synthetic product as the target compound. The synthesis process has the advantages of simple process, safe production, mild reaction conditions, lower production cost, environment friendliness and high product yield.