Controlled hydrolysis of AlMe to tetramethylalumoxane and a new look at incipient adducts with water

We present an efficient route to tetramethylalumoxane by the controlled hydrolysis of AlMe 3 in the presence of pyridine. The AlMe 3 (pyr) hydrolysis by 0.5 and 1 equiv. of H 2 O has been followed with real-time 1 H NMR. Based on high-level quantum-chemical calculations, we conclude that hypervalent...

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Published in:Chemical communications (Cambridge, England) England), 2024-08, Vol.6 (7), p.9392-9395
Main Authors: Korona, Krzesimir, Justyniak, Iwona, Pogrebetsky, James, Lemieszka, Marta, Bernatowicz, Piotr, Pietrzykowski, Antoni, Kubas, Adam, Lewi ski, Janusz
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Summary:We present an efficient route to tetramethylalumoxane by the controlled hydrolysis of AlMe 3 in the presence of pyridine. The AlMe 3 (pyr) hydrolysis by 0.5 and 1 equiv. of H 2 O has been followed with real-time 1 H NMR. Based on high-level quantum-chemical calculations, we conclude that hypervalent, pentacoordinate aluminium species are critical in the first steps of hydrolysis. We present a stochiometric route of AlMe 3 hydrolysis to tetramethylalumoxane. Mechanistic studies by NMR and high-level calculations have revealed the role of neutral donor molecules.
ISSN:1359-7345
1364-548X
DOI:10.1039/d4cc03672g