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目的:对目前贝曲西班的合成路线进行优化,以获得可用于工业生产的工艺路线。方法:以5-甲氧基-2-硝基苯甲酸和2-氨基-5-氯吡啶为起始原料制得N-(5-氯-2-吡啶基)-5-甲氧基-2-硝基苯甲酰胺,依次经过硝基还原,酰化,加成反应制得亚氨酸酯,再与二甲胺进行取代反应得到贝曲西班盐酸盐,碱解后成盐得到贝曲西班马来酸盐。结果:所得贝曲西班经HPLC检测纯度达到99.50%以上,总收率为19.63%。结论:该合成路线操作简单,收率较高,产品纯度高,适合工业化生产。
Objective: To optimize the current synthesis route of Bexar in order to obtain a process route that can be used for industrial production. Methods: Starting from 5-methoxy-2-nitrobenzoic acid and 2-amino-5-chloropyridine, N- (5-chloro-2-pyridyl) - nitrobenzamide, followed by nitro reduction, acylation, addition reaction to obtain imidoester, and then with dimethyl amine substitution reaction betrixaban hydrochloride, alkali hydrolysis salt Tramadol maleate. Results: The purity of Bevacizumab was above 99.50% by HPLC, and the total yield was 19.63%. Conclusion: The synthetic route has the advantages of simple operation, high yield, high product purity and suitability for industrialized production.