Dry mechanochemical synthesis of ethenzamide and saccharin 1:1 cocrystal and their evaluation using powder X-ray diffraction and FT-MIR and NIR spectroscopy

Abstract

The purpose of this study was to evaluate effects of dry mechanochemical synthesizes on ethenzamide (EZ) and saccharin (SA) mixture. EZ and SA mixture were evaluated after grinding by mid and near infrared spectroscopy, powder X-ray diffraction (PXRD) and thermal analysis. During the grind, EZ and SA mixture was transformed into their 1:1 cocrystal form. Measurement time course data was applied to multi variate analysis of principal component analysis (PCA). Their cocrystallization could decompose two steps reactions. At first, EZ crystal transform into amorphous phase and their amorphous react with SA molecules after them, hydrogen bond networks were constructed and produce cocrystal was suggested. Combination PCA and several measurement data enable to extract useful chemical information.