甲啶铂的合成、表征、理化性质与晶体结构  

Synthesis,characterization,crystal structure and physicochemical properties of picoplatin

作　　者：普绍平[1,2] 丛艳伟 王庆琨 贝玉祥 栾春芳 李学杰 孙加林[1] 

机构地区：[1]昆明理工大学材料与冶金学院,昆明650093 [2]昆明贵研药业有限公司,昆明650106

出　　处：《中国新药杂志》2010年第17期1605-1608,共4页Chinese Journal of New Drugs

基　　金：云南省技术创新人才培养项目(2004PY-07)

摘　　要：目的:合成铂类抗癌新药甲啶铂,并研究其化学结构、理化性质及晶体结构。方法:以三氯氨铂酸钾为原料合成甲啶铂;采用元素分析、红外、核磁共振、质谱等确征甲啶铂的化学结构;采用BrukerAPEX Ⅱ CCD X-射线单晶衍射仪分析甲啶铂晶体结构;采用《中国药典》2005版收录方法测定甲啶铂的溶解度与熔点。结果:甲啶铂收率达72.74%;所得产品化学结构与理论相符;X-射线单晶衍射分析结果表明甲啶铂中铂(II)离子与氨基和2-甲基吡啶基团中的氮原子以及两个氯原子配位,形成平面正方形结构,R1=0.025 5,wR2=0.087 7;甲啶铂在水和丙酮中极微溶解,乙醇中不溶,微溶于N,N-二甲基甲酰胺,203℃变黑。结论:该甲啶铂合成方法产率高、纯度好、适合规模化生产,所获得的晶体结构数据与文献报道相近,结构表征、理化性质研究数据为全面深入开发甲啶铂打下良好前期工作基础。Obejective： To synthesize picoplatin and characterize its chemical structure.Methods： Picoplatin was synthesized using potassium tricholoramineplatinate as starting material.EA,IR,NMR and MS were used to characterize the chemical structure.X-ray mono-crystalline diffraction instrument was used to characterize the crystal structure.Physicochemical properties parameters were tested using the methods of Chinese Pharmacopoeia（Edition 2005）.Results： The yielding ratio of picoplatin was 72.74%;the chemical structure of the picoplatin sample was consistent with the theoretical one.X-ray diffraction mono-crystal structure analysis showed that in the chemical structure of picoplatin,the Pt（II） atom,coordinated with two N atoms of ammine and 2-picoline and two Cl atoms,is in a square-planar structure.The final R indices R_1=0.025 5,wR_2=0.087 7.Picoplatin was very slightly soluble in water and acetone,insoluble in ethanol and slightly soluble in DMF,and being black at 203 ℃.Conclusion： The new synthesizing way produces high yield and good purity,and is suitable for industrial production;the acquired crystal structure data is similar as the reported ones.The result of chemical structure and physicochemical properties provide a foundation of next-step development of picoplatin.

关 键 词：甲啶铂 合成 表征 晶体结构 

分 类 号：R979.1[医药卫生—药品]