Journal
CRYSTENGCOMM
Volume 15, Issue 37, Pages 7598-7605Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c3ce40938d
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Co-crystals formed by neutral barbituric acid (HBA) molecules and alkaline barbiturate salts have been prepared by solvent-free mechanochemical treatment of solid HBA and alkaline carbonates or bicarbonates. During the reaction the carbonate salts release CO2 and H2O, affording the corresponding barbiturate salts which then co-crystallize with the neutral molecule. These salt co-crystals have the general formula Mx+(BA(-))(x)center dot HBA center dot nH(2)O with (M = Na and K). The compounds can be obtained in a single step, by directly grinding HBA with M2CO3 (4 : 1 ratio) or MHCO3 (2 : 1 ratio), or, alternatively, in two steps: the preparation of the BA salt followed by a further grinding process or crystallization of the resulting salts with a stoichiometric amount of neutral HBA. All compounds have been characterized by means of single-crystal and powder XRD, solid-state NMR (H-1 MAS, C-13 and N-15 CPMAS), vibrational spectroscopies and thermal methods (DSC and TGA). A series of BA(-) salts (either hydrated or anhydrous) of formula Mx+(BA(-))(x)center dot nH(2)O (M = Na, K, Mg and Ca) have also been prepared and reported for comparison.
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