Abstract
Polysiloxane-immobilized phosphine ligand systems have been prepared by hydrolytic condensation of mixtures of Si(OEt) 4 and (R′O) 3Si(CH 2) n PPh 2 ( n = 2, R′ = Me; n = 3, R′ = Et) Polysiloxane-immobilized phosphine-amine and phosphine-thiol ligand systems have been prepared by hydrolytic condensation of mixtures of Si(OEt) 4, (R′O) 3Si(CH 2) n PPh 2 ( n = 2, R′ = Me; n = 3, R′ = Et) and (R′O) 3Si(CH 2) 3X (X = NH 2, R′= Et; X = NHCH 2CH 2NH 2. R′ = Me) or (MeO) 3Si(CH 2) 3SH. In the polysiloxane-immobilized phosphine-amine and phosphine-thiol systems two types of ligand groups are introduced into the polysiloxane matrix during the sol-gel process. Solid-state 13C, 31P and 29Si NMR spectroscopy was used to investigate the structures of the polysiloxane-immobilized ligand systems — e.g., to determine the presence of unhydrolyzed/uncondensed alkoxy groups, to determine the ratios of phosphine to phosphine oxide moieties, to determine details of the silicon-based backbone (relative populations of various types of RSi(-O-) 3 and Si(-O-) 4 moieties) and to establish domain homogeneity throughout a given material.
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