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The effect of milling frequency on a mechanochemical organic reaction monitored by in situ Raman spectroscopy.

Beilstein journal of organic chemistry (2017-11-09)
Patrick A Julien, Ivani Malvestiti, Tomislav Friščić
RÉSUMÉ

We provide the first in situ and real-time study of the effect of milling frequency on the course of a mechanochemical organic reaction conducted using a vibratory shaker (mixer) ball mill. The use of in situ Raman spectroscopy for real-time monitoring of the mechanochemical synthesis of a 2,3-diphenylquinoxaline derivative revealed a pronounced dependence of chemical reactivity on small variations in milling frequency. In particular, in situ measurements revealed the establishment of two different regimes of reaction kinetics at different frequencies, providing tentative insight into processes of mechanical activation in organic mechanochemical synthesis.

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o-Phenylenediamine, Peroxidase substrate, ≥98.0%, powder