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琥珀酸舒马曲坦多晶型的结晶、光谱、晶体学和热分析研究。

Crystallization, spectral, crystallographical, and thermoanalytical studies of succinobucol polymorphism.

机构信息

Department of Chemistry, University of Jyväskylä, 40014 Jyväskylä, Finland; Institute of Chemical Technology, 16628 Prague 6, Czech Republic.

出版信息

J Pharm Sci. 2012 May;101(5):1794-802. doi: 10.1002/jps.23068. Epub 2012 Feb 9.

DOI:10.1002/jps.23068
PMID:22323097
Abstract

Four different polymorphs, A, C, D, and E, of succinobucol were isolated and characterized by means of solid-state nuclear magnetic resonance spectroscopy, single crystal and powder X-ray diffraction, differential scanning calorimetry, thermogravimetry, and attenuated total reflection-infrared spectroscopy. From a number of experiments, the same polymorphs (C, D, and E) and an equilibrium phase mixture B consisting of polymorphs C and D were repeatedly gained using different solvents or their mixtures. Although polymorph A was obtained directly from recrystallization only on few occasions, polymorphs C, D, and E proved to be metastable kinetic polymorphs, which slowly transform to a thermodynamically more stable form A during long-term storage. The single-crystal structures of polymorph C and D were determined by X-ray single-crystal diffraction.

摘要

四种不同的琥珀酰布醇多晶型物 A、C、D 和 E 通过固态核磁共振波谱、单晶和粉末 X 射线衍射、差示扫描量热法、热重分析和衰减全反射-红外光谱进行了分离和表征。通过多项实验,使用不同溶剂或其混合物,反复得到相同的多晶型物(C、D 和 E)和由多晶型物 C 和 D 组成的平衡相混合物 B。尽管多晶型物 A 仅在少数情况下直接从重结晶中获得,但多晶型物 C、D 和 E 被证明是亚稳动力学多晶型物,在长期储存过程中它们会缓慢地转变成热力学上更稳定的多晶型物 A。多晶型物 C 和 D 的单晶结构通过 X 射线单晶衍射确定。

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