Journal
JOURNAL OF ORGANOMETALLIC CHEMISTRY
Volume 621, Issue 1-2, Pages 231-241Publisher
ELSEVIER SCIENCE SA
DOI: 10.1016/S0022-328X(00)00843-3
Keywords
hydridoaluminates; binaphtholato aluminates; NMR; X-ray structures
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The reaction of LiAlH4 with ROH (R = Pr-i, Bu-t) and binaphthol (binapH(2)) in a 1:1:1 ratio in ether-THF yields a dominant Al-27-NMR signal which is attributed to LiAlH(OR)(binap) (1). However, within a short time more signals emerge, and, depending on concentration, temperature and time the following compounds were isolated and characterized by X-ray structure analysis: LiAlH2(binap).2THF (2.2THF), Li3Al(binap)(3).6THF (3.6THF), Li2Al2(binap)(4).4THF (4.4THF), LiAl(OR)(2)binap.2THF (5.2THF), LiAl(OR)(2)binap.PMDTA (SPMDTA) and Li,ALH(binap)(2).4THF (6.4THF). Moreover, the alane derivative AlH(binap)THF (6), which is dimeric in the solid state, has been prepared and its structure determined. Thus, ligand redistribution is a typical feature for the Noyori reagent in consonance with other lithium alkoxyaluminates. The active species of Noyori's reagent still needs to be discovered. (C) 2001 Elsevier Science B.V. All rights reserved.
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