tert-butoxysilanols as model compounds for labile key intermediates of the sol-gel process: Crystal and molecular structures of (t-BuO)3SiOH and HO[(t-BuO)2SiO]2H

Abstract

The tert-butoxychlorosilanes (t-BuO)3SiCl (1), (t-BuO)2SiCl2O (2), and [(t-BuO)2SiCl]2O (3) were prepared by the reaction of SiCl4 or (Cl3Si)2O with t-BuOK. Subsequent hydrolysis afforded the tert- butoxysilanols (t-BuO)3SiOH (4), (t-BuO)2Si(OH)2 (5), HO[(t-BuO)2SiO]2H (6) in high yields. The controlled condensation of 2 and 5 provided HO[(t-BuO)2SiO]3H (7) in reasonable yields. The tendency of 4-7 to undergo self-condensation is small, thus enabling their characterization in solution and in the solid state by 29Si NMR spectroscopy, IR spectroscopy and electrospray mass spectrometry, and in the case of 4 and 6 also by X-ray diffraction. The key feature of the crystal structures is the incorporation of tert-butoxy groups into the hydrogen bonding. The results obtained are discussed in relation to the sol-gel process. Copyright © 2002 John Wiley & Sons, Ltd.