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Reaction of an Al‐centered anion with toluene proceeded to form C−H cleaved product with a perfect meta‐selectivity and a relatively small kinetic isotope effect (KIE, kH/kD=1.51). DFT calculations suggested a two‐step reaction mechanism and electronically controlled meta‐selectivity arising from the electron‐donating methyl group. The reaction with other mono‐substituted arenes was also investigated.
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