| 摘要: |
| 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、13C-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。 |
| 关键词: 维达列汀 杂质 合成 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.04.011 |
| 分类号:R914.5 |
| 基金项目: |
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| Synthesis of the Main Impurities of Vildagliptin |
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PENG Jiaxun1, MAO Yu2
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1.Hunan Institute of Engineering, Xiangtan 411101, China;2.Changsha Rongguangda Biological Technology Co., Ltd., Changsha 410013, China
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| Abstract: |
| OBJECTIVE To conduct the quality control of an oral antidiabetic vildagliptin, three impurities recorded in quality specifications were prepared.METHODS Impurity A was obtained from vildagliptin(1) by ring-closure reaction. Impurity B was generated in impurity A by hydrolytic reaction. Impurity B and impurity C could be also synthesized from vildagliptin(1), via hydrolytic reaction, esterification and ring-closure reaction. RESULTS The chemical structures of the three impurities were confirmed by LC-MS, 1H-NMR and 13C-NMR. The purities were >97% as determined by HPLC. CONCLUSION The synthesized impurities can be used as the standard substances in the quality control of vildagliptin. |
| Key words: vildagliptin impurity synthesis |
