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

The synthetic method for preparing N-(3-hydroxypropyl) 3α,12α-dihydroxy-5βcholan-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 C-CP/MAS-NMR and IR spectroscopy, thermogravimetry, differential scanning calorimetry and by powder and single crystal x-ray crystallography. In addition, theoretical C-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 · H2O, crystallizes in orthorhombic space group P212121 with cell parameters: a = 7.1148(2), b = 18.1775(5), c = 20.1813(6), Z = 4.