J. Beckmann, D. Dakternieks,, A. Duthie
2003
Citations
1
Influential Citations
33
Citations
Journal
Applied Organometallic Chemistry
Abstract
The tert-butoxychlorosilanes (t-BuO)3SiCl (1), (t-BuO)2SiCl2 (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.