Studies of the Ligand Effect on the Synthesis of Dialuminoxanes by Various β-Diketiminato Ligands
journal contribution
posted on 2016-02-22, 05:29 authored by Ying Yang, Haipu Li, Chen Wang, Herbert W. RoeskyReactions of LH (L = HC[C(Me)N(2,6-Me2C6H3)]2) with MenAlCl3–n in diethyl ether
afforded the adducts
LH·AlMen(Cl)3–n (n = 2, 3; 1, 4; 0, 5) in good yields. Treatment of 3 at elevated temperatures in toluene resulted in LAlMeCl (2) by intramolecular elimination of methane. The controlled hydrolysis
of LAlMeCl (2) with equimolar amounts of water in the
presence of N-heterocyclic carbene (NHC) gave a mixture of [LAl(Me)]2(μ-O) (7) and dimeric [LAlMe(μ-OH)]2 (8). A convenient route for the preparation
of [LAlMe(μ-OH)]2 (8) was the NHC-assisted
controlled hydrolysis of LAlMeI (9). Stepwise hydrolysis
of LAlH2 (11) gave dialuminoxane hydride [LAl(H)]2(μ-O) (12) and dialuminoxane hydroxide
[LAl(OH)]2(μ-O) (13), respectively.
Anhydrous treatment of LAlCl2 (1) or LAlMeCl
(2) with Ag2O afforded chlorinated dialuminoxane
[LAl(Cl)]2(μ-O) (14) and [LAl(Me)]2(μ-O) (7), respectively.
