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目的研究平喘药甲磺司特的合成工艺。方法以丙烯酸甲酯为原料,经加成、水解和氯代反应得到3-甲硫基丙酰氯;以对硝基苯酚为原料,经成醚、开环及还原反应制得4-(3-乙氧基-2-羟基丙氧基)苯胺,中间体3-甲硫基丙酰氯与4-(3-乙氧基-2-羟基丙氧基)苯胺的酰化产物经对甲苯磺酸甲酯甲基化,制得目标物甲磺司特。结果与结论目标化合物的结构经核磁共振氢谱、元素分析、红外光谱、质谱等确证。简化后的合成工艺,总收率由文献报道的4.5%提高到9.97%(以对硝基苯酚计),该合成路线操作简单,更适合工业化生产。
Objective To study the synthetic process of asthma drug asthma. Methods Methyl acrylate was used as the starting material to obtain 3-methylthiopropionyl chloride by addition reaction, hydrolysis and chlorination reaction. Using p-nitrophenol as starting material, 4- (3- Ethoxy-2-hydroxypropoxy) aniline, the acylation product of the intermediate 3-methylthiopropionyl chloride and 4- (3-ethoxy-2-hydroxypropoxy) aniline with p-toluenesulfonic acid methyl Ester methylation, to obtain the target metsulfuron. Results and Conclusion The structures of target compounds were confirmed by 1H NMR, elemental analysis, IR, MS. After the simplified synthesis process, the total yield increased from 4.5% reported in the literature to 9.97% (based on p-nitrophenol). The synthetic route is simple to operate and more suitable for industrial production.