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[目的]寻找一条合成4-甲基-5-咪唑甲酸乙酯的新工艺路线。[方法]以乙酰乙酸乙酯、磺酰氯与甲酰胺为原料,采用一锅法合成一种用途广泛的多功能单体4-甲基-5-咪唑甲酸乙酯。[结果]通过实验,确定了一条合成4-甲基-5-咪唑甲酸乙酯的新工艺:以二氧六环为溶剂,环化时反应温度为120℃,反应时间为4 h,n(乙酰乙酸乙酯)∶n(磺酰氯)∶n(甲酰胺)为1∶1∶2,在该条件下,4-甲基-5-咪唑甲酸乙酯的产率为70%。[结论]该方法路线简单,原料易得,适合工业化生产。
[Objective] The research aimed to find a new route for the synthesis of ethyl 4-methyl-5-imidazolecarboxylate. [Method] With ethyl acetoacetate, sulfonyl chloride and formamide as raw materials, a one - pot synthesis of a versatile multifunctional monomer ethyl 4 - methyl - 5 - imidazole ethyl. [Result] Through the experiment, a new process for the synthesis of ethyl 4-methyl-5-imidazolecarboxylate was established. The reaction temperature was 120 ℃ and the reaction time was 4 h with dioxane as solvent. The reaction time was n Ethyl acetoacetate): n (sulfonyl chloride): n (formamide) was 1: 1: 2. Under this condition, the yield of ethyl 4-methyl-5-imidazolecarboxylate was 70%. [Conclusion] The method has simple route, easy to get raw materials and suitable for industrialized production.