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目的对脱氢环氧甲基醌霉素(DHMEQ)的合成工艺进行改进研究。方法以阿司匹林和2,5-二甲氧基苯胺为起始原料,经缩合、碘苯二乙酯氧化、过氧化氢环氧化、酸催化脱缩酮保护、Na BH4还原成目标化合物,关键的环氧化步骤采用HPLC监控并通过调整反应条件进行工艺优化。结果剔除了柱色谱步骤,优化后制得的目标化合物质量分数为99.4%,工艺总收率为30.0%。结论 DHMEQ的合成工艺改进后操作简便,产品质量可控,适合工业化生产。
Objective To improve the synthesis of dehydroepoxymethylquinoximin (DHMEQ). Methods Aspirin and 2,5-dimethoxyaniline were used as starting materials. After condensation, oxidation of iodobenzene diethyl ester, hydrogen peroxide epoxidation and acid-catalyzed deketalization, Na BH4 was reduced to the target compound The epoxidation step was monitored by HPLC and the process was optimized by adjusting the reaction conditions. Results The column chromatography step was omitted. After optimization, the mass fraction of the target compound was 99.4% and the total yield was 30.0%. Conclusion DHMEQ synthesis process is simple and easy to operate, product quality controllable, suitable for industrial production.