Further Characterization of the Solid Forms of Iopanoic Acid and its Enantiomers
作者:
Davide Pitrè,
Marco De Amici,
Mario Colombo,
Gian Gualberto Gallo,
Marino Nebuloni,
期刊:
Archiv der Pharmazie
(WILEY Available online 1992)
卷期:
Volume 325,
issue 7
页码: 385-388
ISSN:0365-6233
年代: 1992
DOI:10.1002/ardp.19923250703
出版商: WILEY‐VCH Verlag
数据来源: WILEY
摘要:
AbstractThe enantiomers of iopanoic acid were purified by crystallization and characterized by optical rotation, DSC, IR spectra, X‐ray powder diffraction, and chiral HPLC. (‐R)‐enantiomer: [α]20D = −6.1°, mp. = 165.4°C; (+S)‐enantiomer: [α]20D = + 6.2°, mp. = 165.6°C. The IR spectra and X‐ray patterns are fingerprints. Chiral HPLC (isocratic method, mobile phase: ethanol/n‐hexane, 2/98 with 0.5% acetic acid) gave a resolution = 0.98 and a 99.6% recovery.From X‐ray and thermal analyses the racemate FormI, mp. = 153.8°C, resulted to be a racemic compound. The binary phase diagram between the enantiomers and the racemic compound was constructed from the phase transition temp. obtained by DSC heating curves of appropriate mixtures. At a given enantiomer ratio (71/29) a eutectic compound, mp. = 144.7°C, is formed. In the range 88–100% a solid solution between t
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