富马酸卢帕替芬杂质C制备工艺和结构确证
Preparation process and structure confirmation of impurity C of rupatifen fumarate
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摘要: 以卢帕替芬为原料，经溴代丁二酸亲核取代反应，分离纯化获取高纯度的杂质C化合物，运用IR、UV、MS、1H NMR、13C NMR、DEPT135°、HSQC、HMBC、1H-1HCOSY等技术手段对其结构进行确证。本研究制备的杂质C制备工艺简单、条件温和、易于获得，纯度99.0%，收率25%～30%；并且样品经结构确证符合目标化合物。杂质C的制备和结构确证为新药富马酸卢帕替芬原料及制剂的杂质研究提供了杂质C对照品，为富马酸卢帕替芬质量控制提供了理论依据。Abstract: The high-purity impurity C was isolated and purified from a new anti-allergic drug, rupatifen, by nucleophilic substitution reaction with bromobutaric acid, and its structure was confirmed by IR, UV, MS, 1H NMR, 13C NMR, DEPT135°,HSQC, HMBC, and 1H-1HCOSY. The preparation process of impurity C in this study was simple and easy to obtain under mild conditions, with the purity of 99.0% and the yield of 25%-30%;and the sample met the target compound by structural confirmation. The preparation process and structure confirmation provided sufficient impurity C reference substance for impurity research of raw materials and preparations of rupatifen fumarate, which laid a solid foundation for quality research of new drugs.
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