School of Chemistry and Chemical Engineering, Central South University, 410083 Changsha, PR China.
Inorg Chem. 2012 Feb 20;51(4):2204-11. doi: 10.1021/ic2021879. Epub 2012 Feb 9.
Reactions of LH (L = HCC(Me)N(2,6-Me(2)C(6)H(3))) with Me(n)AlCl(3-n) in diethyl ether afforded the adducts LH·AlMe(n)(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)(μ-O) (7) and dimeric LAlMe(μ-OH) (8). A convenient route for the preparation of LAlMe(μ-OH) (8) was the NHC-assisted controlled hydrolysis of LAlMeI (9). Stepwise hydrolysis of LAlH(2) (11) gave dialuminoxane hydride LAl(H)(μ-O) (12) and dialuminoxane hydroxide LAl(OH)(μ-O) (13), respectively. Anhydrous treatment of LAlCl(2) (1) or LAlMeCl (2) with Ag(2)O afforded chlorinated dialuminoxane LAl(Cl)(μ-O) (14) and LAl(Me)(μ-O) (7), respectively.
LH（L=HCC(Me)N(2,6-Me(2)C(6)H(3))）与 Me(n)AlCl(3-n)（n=2,3；1,4；0,5）在乙醚中的反应以高产率得到了 LH·AlMe(n)(Cl)(3-n)（n=2,3；1,4；0,5）的加合物。在甲苯中，3 在高温下处理导致通过甲烷的分子内消除生成 LAlMeCl（2）。在 N-杂环卡宾（NHC）存在下，用等摩尔量的水对 LAlMeCl（2）进行受控水解，得到LAl(Me)(μ-O)（7）和二聚体LAlMe(μ-OH)（8）的混合物。制备LAlMe(μ-OH)（8）的一种方便方法是 NHC 辅助的 LAlMeI（9）的受控水解。LAlH(2)（11）的逐步水解分别得到二铝氧烷氢化物LAl(H)(μ-O)（12）和二铝氧烷氢氧化物LAl(OH)(μ-O)（13）。无水处理 LAlCl(2)（1）或 LAlMeCl（2）与 Ag(2)O 分别得到氯化二铝氧烷LAl(Cl)(μ-O)（14）和LAl(Me)(μ-O)（7）。
