Study and characterization of crystalline hydrate/polymorph forms of 5,11-dihydro-11-ethyl-5-methyl-8-(2-(1-oxido-4-quinolinyl)ethyl-6H-dipyrido(3,2-B:2′,3′-E)(1,4)diazepin-6-one by solid-state NMR and solution NMR
| Autor: | Daniel L. Norwood, Carl A. Busacca, Scot Campbell, Varsolona Richard J, Cerreta Michael Kenneth, John A. Smoliga, Nina C. Gonnella |
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| Rok vydání: | 2010 |
| Předmět: |
Magnetic Resonance Spectroscopy
Pyridines Stereochemistry Clinical Biochemistry Solid-state Pharmaceutical Science Crystallography X-Ray Analytical Chemistry Crystallinity Drug Discovery Technology Pharmaceutical Spectroscopy Molecular Structure Chemistry Water Azepines Carbon-13 NMR Crystallography Solid-state nuclear magnetic resonance Polymorphism (materials science) Anhydrous Reverse Transcriptase Inhibitors Crystallization Hydrate Powder Diffraction Powder diffraction |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 51:1047-1053 |
| ISSN: | 0731-7085 |
| Popis: | A novel inhibitor of reverse transcriptase was studied by solid-state NMR. Three phases of the compound were examined which included the dihydrate and two anhydrous polymorphs (Form I and Form III). By correlating 1 H and 13 C solution NMR with the solid-state 13 C NMR CP/MAS and CPPI spectral editing experiments, comparative 13 C assignments were made for each phase. Polymorphs of Form I and Form III and the dihydrate were easily distinguished based upon chemical shift patterns of the carbon resonances. The 1 H spin-lattice relaxation times were also measured for each phase which provided information on the mobility and relative crystallinity. The 13 C ssNMR spectrum of Form I showed the presence of a minor component identified as the dihydrate. Weight/percent quantitation of major and minor components in Form I was obtained from integrated intensities of a 50:50 mixture containing weighed amounts of Form I and the pure dihydrate. Comparison of the ssNMR and X-ray powder diffraction techniques is discussed. |
| Databáze: | OpenAIRE |
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