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

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 usi...

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Autores principales: Kulla, Hannes, Greiser, Sebastian, Benemann, Sigrid, Rademann, Klaus, Emmerling, Franziska
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2016
Materias:
Article
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6274108/
https://www.ncbi.nlm.nih.gov/pubmed/27428942
http://dx.doi.org/10.3390/molecules21070917
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author Kulla, Hannes
Greiser, Sebastian
Benemann, Sigrid
Rademann, Klaus
Emmerling, Franziska
author_facet Kulla, Hannes
Greiser, Sebastian
Benemann, Sigrid
Rademann, Klaus
Emmerling, Franziska
author_sort Kulla, Hannes
collection PubMed
description 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.
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spelling pubmed-62741082018-12-28 In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid Kulla, Hannes Greiser, Sebastian Benemann, Sigrid Rademann, Klaus Emmerling, Franziska Molecules Article 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. MDPI 2016-07-14 /pmc/articles/PMC6274108/ /pubmed/27428942 http://dx.doi.org/10.3390/molecules21070917 Text en © 2016 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC-BY) license (http://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Kulla, Hannes
Greiser, Sebastian
Benemann, Sigrid
Rademann, Klaus
Emmerling, Franziska
In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid
title In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid
title_full In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid
title_fullStr In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid
title_full_unstemmed In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid
title_short In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid
title_sort in situ investigation of a self-accelerated cocrystal formation by grinding pyrazinamide with oxalic acid
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6274108/
https://www.ncbi.nlm.nih.gov/pubmed/27428942
http://dx.doi.org/10.3390/molecules21070917
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