Crystallization, spectral, crystallographical, and thermoanalytical studies of succinobucol polymorphism.
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.
Department of Chemistry, University of Jyväskylä, 40014 Jyväskylä, Finland; Institute of Chemical Technology, 16628 Prague 6, Czech Republic. jurcekondrej@gmail.com
Ondřej
O
Jurček
Manu
M
Lahtinen
Zdeněk
Z
Wimmer
Pavel
P
Drašar
Erkki
E
Kolehmainen
D002152:Calorimetry, Differential Scanning; D003460:Crystallization; D018360:Crystallography, X-Ray; D009682:Magnetic Resonance Spectroscopy; D008958:Models, Molecular; D033362:Powder Diffraction; D011341:Probucol / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D013055:Spectrophotometry, Infrared; D013818:Thermogravimetry
C471047:succinobucol; D011341:Probucol