Novel diaminoaluminum halides and a diaminoaluminum hydride: 1,3,2-Diazaalumina-[3]ferrocenophanes

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• 作者：Bernd Wrackmeyer ; Elena V. Klimkina ; Wolfgang Milius
• 关键词：Aluminum amides ; [3]Ferrocenophanes ; NMR ; X-ray structure
• 刊名：Polyhedron
• 出版年：2007
• 出版时间：31 August 2007
• 年：2007
• 卷：26
• 期：14
• 页码：3496-3504
• 全文大小：560 K

文摘

The dilithiated derivative 2 of 1,1′-bis(trimethylsilylamino)ferrocene (1) reacts with the pyridine adducts of the aluminum trihalides AlX₃ (X = Cl, Br, I) to give the respective 1,3,2-diazaalumina-[3]ferrocenophanes (4b, c, d) as pyridine adducts. The fluoride 4a could not be obtained in this way. The reaction of 1,1′-bis(trimethylsilylamino)ferrocene (1) with the dimethyl(ethyl)amine- or pyridine adduct of aluminium trihydride gave the 1,3,2-diazaalumina-[3]ferrocenophanes (5) and (6) as the amine and pyridine adducts, respectively. Treatment of 5 with trimethyltin fluoride afforded the adduct 7 with an Al–F function. Addition of pyridine converted 7 into the desired pyridine adduct of the fluoride (4a). The molecular structures of the pyridine adducts 4a, 4b, 4c and 6 were determined by X-ray analysis. The pyridine is in the trans-position relative to the N–Si bond vectors, and temperature dependent solution-state NMR spectra prove that prominent structural features are retained in solution.