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

Molecules

Arto Valkonen¹  Erkki Kolehmainen²  Manu Lahtinen²  Elina Sievänen²  Virpi Noponen²  Minna Tolonen² 

[1] id="af1-molecules-12-02161">Department of Chemistry, University of Jyväskylä, PO. Box 35, FIN-40014 University of Jyväskylä, Finla

关键词: Bile acids;    ¹³C-CP/MAS-NMR spectroscopy;    crystallography;    thermal analysis;    solid state structure;   

DOI  :  10.3390/12092161

来源: mdpi

【 摘 要 】

The synthetic method for preparing N-(3-hydroxypropyl) 3α,12α-dihydroxy-5β-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 · H₂O, crystallizes in orthorhombic space group P2₁2₁2₁ with cell parameters: a = 7.1148(2), b = 18.1775(5), c = 20.1813(6), Z = 4.

【 授权许可】

Unknown   
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