Norbert Emig, Hanh Nguyen, H. Krautscheid
Jul 15, 1998
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Quality indicators
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Organometallics
Abstract
The dilithium salts of N,N‘,N‘‘-tris(trimethylsilyl)diethylenetriamine (1), N-methyl-N‘,N‘‘-bis(trimethylsilyl)diethylenetriamine (2), and N-methyl-N‘,N‘‘-bis(diisopropyl)diethylenetriamine (3) reacted in THF, at −40 °C, with AlCl3 affording monomeric aluminum chloride derivatives 4 (55% yield), 5 (76% yield), and 6 (71% yield), respectively. Addition of 1 equiv of AlMe3 to the amine 2 gave rise to the five-coordinate dimethylaluminum derivative 9 (67% yield); heating a toluene solution of 9 overnight at 80 °C induces a loss of methane giving rise to the four-coordinate methylaluminum compound 10 (50% yield). The amine 2 also reacted at low temperature with LiAlH4 affording derivative 11 (38% yield). Compounds 4−6 reacted subsequently in toluene with 1 equiv of HCl and 1 equiv of AlCl3 to afford the first chiral tetracoordinated aluminum cations 12 (94% yield), 13 (93% yield), and 14 (90% yield), respectively. Single-crystal X-ray diffraction studies of derivatives 4, 5, 8, 10, 11, 12, and 15 have been ca...