盐酸去甲金霉素的单晶制备及其结构表征  

Single crystal culture and structure characterization of demeclocycline hydrochloride

作　　者：朱兰芳[1,2] 范钢[2] 王文斌 王董 吴孔涛 高浩凌 ZHU Lan-fang;FAN Gang;WANG Wen-bin;WANG Dong;WU Kong-tao;GAO Hao-ling(Xinchang Pharmaceutical Factory,Zhejiang Medicine Co.,Ltd.,Shaoxing 312500,China;Research&Development Center,Zhejiang Medicine Co.,Ltd.,Shaoxing 312300,China)

机构地区：[1]浙江医药股份有限公司新昌制药厂,浙江绍兴312500 [2]浙江医药股份有限公司研究院,浙江绍兴312300

出　　处：《现代药物与临床》2023年第3期547-552,共6页Drugs & Clinic

基　　金：工业与信息化部化学原料药环保安全技术服务平台项目(2020-0107-3-1)。

摘　　要：目的培养盐酸去甲金霉素的单晶,进行结构表征。方法用水培养单晶,使用热重法(TGA)、粉末X射线衍射(PXRD)、单晶X射线衍射(SXRD)检测分析。结果制备的盐酸去甲金霉素为无色粒状晶体,晶胞属于单斜晶系,空间群为P2_(1),分子式为C_(2_(1))H_(2_(1))ClN_(2)O_(8)·HCl·3H_(2)O,相对分子质量为555.35,晶体密度为1.593 mg/mm^(3),绝对构型为S,S,S,S,S构型。结论证明了盐酸去甲金霉素的立体构型,培养的晶体晶型为三水合物。Objective To cultivate single crystal of demeclocycline hydrochloride,and to characterize its structure.Methods Cultivate single crystals with water,and TGA,PXRD,and SXRD were used to detect and analyze.Results Demeclocycline hydrochloride colorless granular crystal was obtained.Crystal in demeclocycline hydrochloride was confirmed to be monoclinic lattice with space group P2_(1).Moreover,the chemical formula and relative molecular mass were C_(2_(1))H_(2_(1))ClN_(2)O_(8)·HCl·3H_(2)O and 555.35.Crystal density were 1.593 mg/mm^(3),and absolute configuration was(S,S,S,S,S).Conclusion Crystal structure of demeclocycline hydrochloride is characterized,and the crystal form is demeclocycline hydrochloride trihydrate.

关 键 词：盐酸去甲金霉素 单晶 制备 热重法 粉末X射线衍射 单晶X射线衍射 结构表征 

分 类 号：R914[医药卫生—药物化学]