6533b834fe1ef96bd129e0eb

RESEARCH PRODUCT

Structural, Thermoanalytical and Molecular Modeling Studies on N-(3-hydroxypropyl) 3a,12a-Dihydroxy-5b-cholan-24-amide and Its Monohydrates

Minna TolonenElina SievänenManu LahtinenArto ValkonenReijo KauppinenVirpi NoponenErkki Kolehmainen

subject

Models MolecularMagnetic Resonance Spectroscopysolid state structure.termoanalyysiPharmaceutical ScienceInfrared spectroscopy13C-CP/MAS-NMR spectroscopy13C-CP/MAS-NMR spektroskopiaFull Research PaperAnalytical ChemistryCrystallcsh:QD241-441Differential scanning calorimetrylcsh:Organic chemistryX-Ray DiffractionDrug Discoverykiinteän tilan rakenneSolid state structurePhysical and Theoretical ChemistrycrystallographyCarbon Isotopeskristallografiathermal Bile acidsCalorimetry Differential ScanningChemistryHydrogen bondOrganic ChemistryTemperatureWaterHydrogen BondingkidetiedeAmidesBile acidsCrystallographysappihapotChemistry (miscellaneous)X-ray crystallographyThermogravimetryAnhydrousCholanesMolecular MedicineOrthorhombic crystal systemSingle crystalthermal analysis

description

The synthetic method for preparing N-(3-hydroxypropyl) 3 alpha,12 alpha-dihydroxy-5 beta-cholan-24-amide can lead to formation of at least three different crystal forms - an anhydrous compound and two monohydrates. The structural and thermal properties of these forms have been characterized by 13C-CP/MAS-NMR and IR spectroscopy, thermo- gravimetry, differential scanning calorimetry and by powder and single crystal x-ray crystallography. In addition, theoretical 13C-NMR chemical shift calculations were also performed for the anhydrous compound and for the first monohydrate, starting from single crystal structures and the structures of these species have now been verified. The first monohydrate, C27H47NO4 x H2O, crystallizes in orthorhombic space group P2(1)2(1)2(1) with cell parameters: a = 7.1148(2), b = 18.1775(5), c = 20.1813(6), Z = 4.

yearjournalcountryeditionlanguage
2007-09-12
http://urn.fi/URN:NBN:fi:jyu-201612135067