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Methylalumoxane (MAO) ionizes highly selectively in the presence of octamethyltrisiloxane (OMTS) to generate [Me 2 Al·OMTS] + [(MeAlO) 16 (Me 3 Al) 6 Me] - . We can take advantage of this transformation to examine the reactivity of a key component of MAO using electrospray ionization mass spectrometry (ESI-MS), and here we describe the reactivity of this pair of ions with other trialkyl aluminum (R 3 Al) components. Using continuous injection methods, we found E 3 Al to exchange much faster and extensively at room temperature in fluorobenzene ( ½ ∼2 s, up to 25 exchanges of Me for Et) than iBu 3 Al ( ½ ∼40 s, up to 11 exchanges) or Oc 3 Al ( ½ ∼200 s, up to 7 exchanges). The exchanges are reversible and the methyl groups on the cation are also observed to exchange with the added R 3 Al species. These results point to the reactive components of MAO having a structure that deviates significantly from the cage-like motifs studied to date.

Modifying methylalumoxane via alkyl exchange