Caira Mino R, Bettinetti Giampiero, Sorrenti Milena, Catenacci Laura
Department of Chemistry, University of Cape Town, Rondebosch 7701, South Africa.
J Pharm Sci. 2007 May;96(5):996-1007. doi: 10.1002/jps.20934.
The isolation and physicochemical characterization of four crystalline modifications of brodimoprim (5-[(4-bromo-3,5-dimethoxyphenyl)methyl]-2,4-pyrimidinediamine, hereinafter BMP), a structural analog of trimethoprim (TMP), are reported. These phases include an unsolvated form of BMP, a hemihydrate (BMP 0.5H(2)O), a 1:1 solvate containing isopropanol (BMP C(3)H(7)OH(iso)), and a hemichloroformate (BMP 0.5CHCl(3)). Unsolvated BMP was isolated both by recrystallization from a range of common solvents as well as by thermal decomposition of the above solvates and no evidence for polymorphism was found. PXRD data indicated that the three solvates crystallize in different arrangements. Data from thermal analysis (thermogravimetry (TGA), hot stage microscopy (HSM), differential scanning calorimetry (DSC)) of the solvates containing water and iso-propanol were interpreted on the basis of their single-crystal X-ray structures which revealed that the modes of solvent inclusion in BMP 0.5H(2)O and BMP C(3)H(7)OH(iso) may be described as 'isolated site' and 'lattice channel' type inclusions, respectively.
报告了甲氧苄啶(TMP)的结构类似物溴莫普明(5-[(4-溴-3,5-二甲氧基苯基)甲基]-2,4-嘧啶二胺,以下简称BMP)四种晶型的分离及其物理化学特性。这些晶相包括BMP的非溶剂化形式、半水合物(BMP 0.5H₂O)、含异丙醇的1:1溶剂化物(BMP C₃H₇OH(iso))和半氯甲酸酯(BMP 0.5CHCl₃)。通过从一系列常用溶剂中重结晶以及上述溶剂化物的热分解,分离得到了非溶剂化的BMP,未发现多晶型现象的证据。粉末X射线衍射(PXRD)数据表明,这三种溶剂化物以不同的排列方式结晶。基于含水和异丙醇的溶剂化物的单晶X射线结构,对其热分析(热重分析(TGA)、热台显微镜(HSM)、差示扫描量热法(DSC))数据进行了解释,结果表明,BMP 0.5H₂O和BMP C₃H₇OH(iso)中溶剂的包合模式可分别描述为“孤立位点”和“晶格通道”型包合。