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目的为了加强抗糖尿病药物维达列汀原料药的质量控制,合成了维达列汀的3个特定杂质。方法维达列汀(1)经闭环反应制得杂质A;以杂质A为原料经水解反应制得杂质B;维达列汀(1)经水解反应、酯化反应和闭环反应制得杂质B和杂质C。结果合成的3种杂质的结构经过~1H-NMR、~(13)C-NMR和LC-MS确证,纯度经HPLC检测>97%。结论合成的3种杂质可以作为维达列汀原料药质量控制的杂质对照品。
Objective To improve the quality control of the antidiabetic drug vildagliptin, three specific impurities of vildagliptin have been synthesized. Method Vildagliptin (1) was prepared by closed-loop reaction of impurities A; impurities A as raw material by hydrolysis reaction to obtain impurities B; Vildagliptin (1) by hydrolysis, esterification and ring closure reaction impurities B And impurity C Results The structures of the three impurities synthesized were confirmed by ~ 1H-NMR, ~ (13) C-NMR and LC-MS. The purity of the three impurities was> 97% by HPLC. Conclusion The three impurities synthesized can be used as the reference substance for the quality control of vildagliptin APIs.