卡巴他赛的单晶培养和结构确证.pdf

现代药物与临床 Drugs Clinic 第 31 卷 第 12 期 2016 年 12 月 ·1879 · 卡巴他赛的单晶培养和结构确证 谢寅省，高红云，刘 实 北京美迪康信医药科技有限公司，北京 100012 摘 要：目的 培养卡巴他赛的单晶，进行结构确证。方法 选择适宜的单晶培养用溶剂体系和培养条件。对卡巴他赛单晶 进行 X-射线单晶衍射实验，并进行结构鉴定。结果 醋酸乙酯–正己烷体系 7 d 挥发得到卡巴他赛无色透明柱状结晶。根 据原子坐标、等价温度因子、键长、扭转角数据确定卡巴他赛不对称单位化学计量式为 C49H65NO 16，相对分子质量为 924.02， 3 晶体密度为 1.273 mg/m 。得到卡巴他赛立体结构，证明该晶胞属于单斜晶系，空间群为P2 。结论 采用 X-射线单晶衍射 1 检测卡巴他赛单晶确证了其空间结构，提示合成的卡巴他赛结构正确。 关键词：卡巴他赛；单晶培养；X-射线单晶衍射；结构确证 中图分类号：R914 文献标志码：A 文章编号：1674 - 5515(2016)12 - 1879 - 04 DOI: 10.7501/j.issn.1674-5515.2016.12.002 Single crystal culture and structure confirmation of cabazitaxel XIE Yin-sheng, GAO Hong-yun, LIU Shi Beijing Medconxin Pharmaceutical Technology Limited Company, Beijing 100012, China Abstract: Objective To cultivate single crystal of cabazitaxel, and to establish the structure of cabazitaxel. Methods To selected the best condition by inspecting the different solvent. Suitable solvent and culture conditions were selected to cultivate single crystal. Single crystal of cabazitaxel was studied by X-ray diffraction, and the structure of cabazitaxel was identified. Results Cabazitaxel colorless transparent columnar crystal was obtained in ethyl acetate - hexane solvent system after volatilization for 7 d. According to data of atomic coordinates, equivalent temperature factor, bond distance, and torsion angles, asymmetric unit stoichiometric of 3 cabazitaxel was established as C49H65NO 16, relative molecular mass were 924.02, and crystal density were 1.273 mg/m . Stereostructure of cabazitaxel was obtained, and the crystal was proved to monoc