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

Beilstein J Org Chem. 2017 Oct 18:13:2160-2168. doi: 10.3762/bjoc.13.216. eCollection 2017.

Abstract

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.

Keywords: Raman spectroscopy; green chemistry; mechanism; mechanochemistry; milling; monitoring.