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Molecules 2016, 21(7), 917; doi:10.3390/molecules21070917

In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid

1
Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Str. 11, 12489 Berlin, Germany
2
Department of Chemistry, Humboldt-Universität zu Berlin, Brook-Taylor-Str. 2, 12489 Berlin, Germany
*
Author to whom correspondence should be addressed.
Academic Editors: Koichi Komatsu and Carsten Bolm
Received: 20 June 2016 / Revised: 8 July 2016 / Accepted: 11 July 2016 / Published: 14 July 2016
(This article belongs to the Special Issue Mechanochemistry)
View Full-Text   |   Download PDF [4271 KB, uploaded 14 July 2016]   |  

Abstract

A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes. View Full-Text
Keywords: in situ; cocrystal; mechanochemistry; hydrate; pyrazinamide in situ; cocrystal; mechanochemistry; hydrate; pyrazinamide
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Kulla, H.; Greiser, S.; Benemann, S.; Rademann, K.; Emmerling, F. In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid. Molecules 2016, 21, 917.

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