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Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases (CROSBI ID 240587)

Prilog u časopisu | izvorni znanstveni rad | međunarodna recenzija

Lukin, Stipe ; Stolar, Tomislav ; Tireli, Martina ; Blanco, Maria ; Babić, Darko ; Friščić, Tomislav ; Užarević, Krunoslav ; Halasz, Ivan Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases // Chemistry : a European journal, 23 (2017), 13941-13949. doi: 10.1002/chem.201702489

Podaci o odgovornosti

Lukin, Stipe ; Stolar, Tomislav ; Tireli, Martina ; Blanco, Maria ; Babić, Darko ; Friščić, Tomislav ; Užarević, Krunoslav ; Halasz, Ivan

engleski

Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases

Despite recent advances in real-time and in situ monitoring techniques, a thorough mechanistic understanding of mechanochemical milling reactions is often hindered by the inability of their quantitative evaluation. Here, a tandem approach combining in situ powder X-ray diffraction and Raman spectroscopy enabled quantitative assessment and kinetic analysis of mechanochemical reaction, even when involving new phases of unknown crystal structures, and short-lived intermediates. We also introduce in situ Raman monitoring as a standalone laboratory technique for quantitative assessment of mechanochemical reactions. Our approach is demonstrated on a complex and multi-step mechanochemical cocrystallization of benzoic acid and the model active pharmaceutical ingredient nicotinamide under neat and liquid-assisted grinding, which resulted in complex transformations between four polymorphs. Reaction pathways and polymorph selectivity can be tuned by both the choice of a liquid additive and its amount. Our results provide an important step toward a complete and high-throughput quantitative approach to mechanochemical reaction kinetics and mechanisms, necessary for the development of the mechanistic framework of milling reactions.

quantitative in situ monitoring, monitoring, mechanochemistry, Raman spectroscopy, synchrotron XRD, pharmaceutical cocrystals

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Podaci o izdanju

23

2017.

13941-13949

objavljeno

0947-6539

1521-3765

10.1002/chem.201702489

Povezanost rada

Kemija, Farmacija

Poveznice
Indeksiranost