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  • 1
    ISSN: 1573-904X
    Schlagwort(e): polymorphs ; infrared ; Raman ; solid-state nuclear magnetic resonance ; crystal packing
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract Losartan, an antihypertensive agent in clinical development, was found to exist in two enantiotropic polymorphic forms, a low-temperature stable form (Form I) and a high-temperature stable form (Form II), the temperatures at which they are stable being related to the transition temperature. X-ray powder diffraction patterns indicated differences in the crystal packing of the two forms. The vibrational data from infrared and Raman spectroscopy suggested a subtle change in molecular conformation and crystal packing in the two forms. Solid-state 13C NMR data of the polymorphs concurred with the vibrational data and indicated that, while the observed line widths reflect no major changes in crystallinity, signal multiplicities and chemical shifts do reflect differences in molecular packing in the respective unit cells. Thus, in the absence of crystal-lographic data, useful structural information could be derived from spectroscopic results to identify each of the crystalline forms.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 33 (1995), S. 664-668 
    ISSN: 0749-1581
    Schlagwort(e): 1H NMR ; 13C NMR ; aziridines ; pyramidal nitrogen inversion ; inversion rate constant ; slow exchange spin locking ; 2D exchange spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The slow inversion at pyramidal nitrogen in 2,2-dimethylaziridine was investigated by NMR spectroscopy at 304 K using one-dimensional spin locking methods and two-dimensional exchange spectroscopy. The activation free energy was found to be 17.5 kcal mol-1 (73.2 kJ mol-1) at this temperature. This value represents a lower limit for the unimolecular inversion barrier height as autocatalytic and water-catalyzed inversion pathways can in principle also contribute to the observed rate. The spin locking experiments described employ non-selective pulses and are particularly useful for the quantitative study of slow chemical exchange between nuclei of similar resonance frequency where selective magnetization transfer experiments are difficult or impossible.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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