In situ investigations of a mechanochemical cocrystal formation by X-ray diffraction for two different milling jar materials
- Mechanochemistry has become a valuable method for the synthesis of new materials, especially for pharmaceutical cocrystals. The Advantages of fast reactions in high purity and yield face a lack of understanding the underlying mechanism. Therefore, in situ setups to study mechanochemical reactions have been established. Herein, we present an in situ investigation of the mechanochemical cocrystal formation of pyrazinamide (PZA) with pimelic acid (PM) using synchrotron XRD. Two new polymorphs of PZA:PM (1:1) were synthesized by milling the starting materials in milling jars of different materials. While Form I is only obtained using a steel jar, Form II can be obtained purely in jars made of Perspex. In situ XRD experiments reveal a direct formation of Form II in Perspex and an intermediate formation of Form II in steel jars converting to Form I upon further grinding. Heating experiments and DFT calculations predict that Form II is the thermodynamically more stable polymorph. Therefore,Mechanochemistry has become a valuable method for the synthesis of new materials, especially for pharmaceutical cocrystals. The Advantages of fast reactions in high purity and yield face a lack of understanding the underlying mechanism. Therefore, in situ setups to study mechanochemical reactions have been established. Herein, we present an in situ investigation of the mechanochemical cocrystal formation of pyrazinamide (PZA) with pimelic acid (PM) using synchrotron XRD. Two new polymorphs of PZA:PM (1:1) were synthesized by milling the starting materials in milling jars of different materials. While Form I is only obtained using a steel jar, Form II can be obtained purely in jars made of Perspex. In situ XRD experiments reveal a direct formation of Form II in Perspex and an intermediate formation of Form II in steel jars converting to Form I upon further grinding. Heating experiments and DFT calculations predict that Form II is the thermodynamically more stable polymorph. Therefore, the reaction progress in the steel jar contradicts Ostwald’s rules of stages as the more stable Form II converts into the metastable Form I. Hence, mechanochemistry offers the possibility to synthesize new materials that cannot be obtained using conventional methods.…
Autor*innen: | Hannes Kulla |
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Koautor*innen: | C. Becker, N. Casati, B. Paulus, K. Rademann, Franziska Emmerling |
Dokumenttyp: | Posterpräsentation |
Veröffentlichungsform: | Präsentation |
Sprache: | Englisch |
Jahr der Erstveröffentlichung: | 2017 |
DDC-Klassifikation: | Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten |
Freie Schlagwörter: | Cocrystal; In situ; Mechanochemistry; Milling; Polymorph |
Veranstaltung: | Adlershofer Forschungsforum 2017 |
Veranstaltungsort: | HU-Berlin, Erwin-Schrödinger Zentrum, Germany |
Beginndatum der Veranstaltung: | 10.11.2017 |
Enddatum der Veranstaltung: | 10.11.2017 |
Verfügbarkeit des Dokuments: | Datei im Netzwerk der BAM verfügbar ("Closed Access") |
Datum der Freischaltung: | 17.11.2017 |
Referierte Publikation: | Nein |