Journal
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
Volume 53, Issue 24, Pages 6193-6197Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/anie.201402334
Keywords
in situ techniques; liquid-assisted grinding; mechanochemistry; Raman spectroscopy; reaction mechanisms
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Funding
- Ministry of Science, Education and Sport of the Republic of Croatia [098-0982915-2950, 098-0982904-2953, 098-0982933-2920, 098-0982886-2894]
- Unity through Knowledge Fund (UKF) [7/13]
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Mechanistic understanding of mechanochemical reactions is sparse and has been acquired mostly by stepwise ex situ analysis. We describe herein an unprecedented laboratory technique to monitor the course of mechanochemical transformations at the molecular level in situ and in real time by using Raman spectroscopy. The technique, in which translucent milling vessels are used that enable the collection of a Raman scattering signal from the sample as it is being milled, was validated on mechanochemical reactions to form coordination polymers and organic cocrystals. The technique enabled the assessment of the reaction dynamics and course under different reaction conditions as well as, for the first time, direct insight into the behavior of liquid additives during liquid-assisted grinding.
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