We present an efficient route to tetramethylalumoxane by the controlled hydrolysis of AlMe in the presence of pyridine. The AlMe(pyr) hydrolysis by 0.5 and 1 equiv. of HO has been followed with real-time H NMR. Based on high-level quantum-chemical calculations, we conclude that hypervalent, pentacoordinate aluminium species are critical in the first steps of hydrolysis.
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