通过将吡嗪酰胺与草酸研磨进行自加速共晶形成的原位研究。
In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid.
作者信息
Kulla Hannes, Greiser Sebastian, Benemann Sigrid, Rademann Klaus, Emmerling Franziska
机构信息
Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Str. 11, 12489 Berlin, Germany.
Department of Chemistry, Humboldt-Universität zu Berlin, Brook-Taylor-Str. 2, 12489 Berlin, Germany.
出版信息
Molecules. 2016 Jul 14;21(7):917. doi: 10.3390/molecules21070917.
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.
通过机械化学方法制备了吡嗪酰胺与草酸的新型共晶体，并通过粉末X射线衍射（PXRD）、拉曼光谱、固态核磁共振光谱、差示热分析-热重分析（DTA-TG）和扫描电子显微镜（SEM）对其进行了表征。基于粉末X射线衍射数据解析了其结构。使用同步加速器PXRD和拉曼光谱联用技术原位研究了该反应的形成途径。使用二水合草酸时，最初的纯研磨通过结晶水的释放转变为快速的自加速液体辅助研磨过程。在这些条件下，两分钟内直接形成了共晶体。
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