摘要
对已有文献报道的合成工艺进行改进,提供关键中间体3-羟基-1,1-环丁烷二羧酸银盐的合成路线,精简操作,缩短反应时间,获得高纯度的目标化合物舒尼铂。采用X射线衍射法(XRD)测定舒尼铂的晶体结构。结构分析结果表明:该配合物在正交晶系空间群C2221中结晶,晶胞参数a=14.446(2)Å,b=19.688(3)Å,c=12.2849(2)Å,V=3654.4(10)Å3,Z=4。在晶体结构中,Pt(II)原子通过和两个N原子及两个O原子配位形成一个略有畸变的正方形结构,且2-异丙基-1,3-二氧戊环呈现出信封式构象,存在混合占位情况,其比例为0.62:0.38。晶体结构中存在多个分子间氢键,形成了一个三维分子网络。
The synthetic method of Suniplatin reported in the literature was optimized,withan aim to provide an efficient process route for the key intermediate silver 3-hydroxy-1,1-cyclobutane-dicarboxylate.The new procedure was streamlined and the reaction time was shortened.As a result,the sample of high-purity Suniplatin was yielded.The crystal structure of Suniplatin was determined by X-ray diffraction.The structural analysis results show that the complex crystallizes in the orthorhombic space group C2221 with a unit cell parameter of a=14.446(2)Å,b=19.688(3)Å,c=12.849(2)Å,V=3654.4(10)Å3,Z=4.In the crystal structure,the Pt(II)atom is coordinated on a slightly distorted square by two N atoms and two O atoms,and 2-isopropyl-1,3-dioxolane displays an envelope conformation with a mixed occupancy of a ratio of 0.62 to 0.38.The multiple intermolecular hydrogen bonds exist in the crystal structure,creating a three dimensional molecular net.
作者
段丽萍
陈晓雪
姜婧
柳知莹
杨志
邓斌
陈雪江
徐红贵
DUAN Liping;CHEN Xiaoxue;JIANG Jing;LIU Zhiying;YANG Zhi;DENG Bing;CHEN Xuejiang;XU Honggui(Yunnan Province Company Key Laboratory for TCM and Ethnic Drug of New Drug Creation,Yunnan Institute of MateriaMedica,Kunming 650500,China;Kunming Institute of Precious Metals,Kunming 650106,China)
出处
《贵金属》
北大核心
2025年第4期57-60,共4页
Precious Metals
基金
国家重大新药创制专项(2009ZX09103-109)
云南省新药开发专项(2014BC010)。
关键词
舒尼铂
合成
单晶
X射线衍射
晶体结构
Suniplatin
synthesis
single-crystal
X-ray diffraction
crystal structure
