6533b7d6fe1ef96bd1266fe9

RESEARCH PRODUCT

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

Erkki KolehmainenPavel DrašarManu LahtinenOndřej JurčekOndřej JurčekZdeněk Wimmer

subject

Models MolecularMagnetic Resonance SpectroscopyCalorimetry Differential ScanningSpectrophotometry InfraredChemistryPharmaceutical ScienceNuclear magnetic resonance spectroscopyCrystallography X-Raylaw.inventionThermogravimetryCrystallographyDifferential scanning calorimetryProbucolPolymorphism (materials science)Solid-state nuclear magnetic resonancelawThermogravimetryCrystallizationCrystallizationta116Single crystalPowder diffractionPowder Diffraction

description

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. © 2012 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 101:1794–1802, 2012

10.1002/jps.23068https://pubmed.ncbi.nlm.nih.gov/22323097