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Structural characterisation of two pharmaceutically important steroids by solid-state NMR

Othman, Abdullah
Harris, Robin K.
Hodgkinson, Paul
Christopher, Elizabeth A.
Lancaster, Robert W.
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EPub Date
Publication Date
2008
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Abstract
Several crystal modifications of two steroids (androsterone and beclomethasone dipropionate) have been characterised by solid-state NMR methods, and the chemical shifts between the different forms compared. The gradual loss of water from androsterone hemihydrate has been monitored by XRPD. The crystal structures are discussed in relation to the NMR data. That of the beclomethasone dipropionate ethyl acetate solvate has been determined for the first time. It is found that there are clear channels containing the ethyl acetate molecules, which are apparently not incorporated by hydrogen bonding. Carbon-13 CPMAS spectra with long contact times and MAS proton spectra are used to show the mobility of ethyl acetate molecules in the BDP solvate. The second-order effect of chlorine on the 13C spectrum of beclomethasone dipropionate monohydrate has been explored by varying the applied magnetic field.
Citation
Othman, A., Harris, R. K., Hodgkinson, P., Christopher, E. A., & Lancaster, R W. (2008). Structural characterisation of two pharmaceutically important steroids by solid-state NMR. New Journal of Chemistry, 32(10), 1796-1806. https://doi.org/10.1039/B803586E
Publisher
Royal Society of Chemistry
Journal
New Journal of Chemistry
Research Unit
DOI
10.1039/b803586e
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PubMed Central ID
Type
Article
Language
en
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ISSN
1144-0546
EISSN
1369-9261
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https://pubs.rsc.org/en/content/articlelanding/2008/nj/b803586e