SYNTHESIS AND SOLID-STATE NMR STRUCTURAL CHARACTERIZATION OF SOME FUNCTIONALIZED POLYSILOXANES

Polysiloxane-immobilized propylamine, diethylpropylamine and trimethyl propylammonium systems, and some other types of ligand systems, have b een prepared. Polysiloxane-immobilized amine and trimethylpropylammoni um chloride materials were made through hydrolytic condensation of Si( OEt)(4) and (EtO)(3)Si(CH2)(3)X, with X=-NH2 or -N+(CH3Cl-. The polysi loxane-immobilized diethylpropylamine ligand system was prepared by th e reaction between the polysiloxane-immobilized 3-chloropropyl system and diethylamine. Polysiloxanes carrying the -CH(2)CO(2)Me group were made by the reaction of methylchloroacetate with polysiloxane-immobili zed amine or thiol ligand systems, S-(CH2)(3)X (where X = -NH2 or -SH; and S represents the polysiloxane backbone). Polysiloxane-immobilized glycinate and iminodiacetate systems were made by the reactions of so dium glycinate or disodium iminodiacetate with the polysiloxane-immobi lized 3-chloropropyl system. Solid-state C-13 and Si-29 NMR spectrosco py, based on cross polarization (CP) and magic-angle spinning (MAS) te chniques, were employed. C-13 NMR results determined that, in the abov e-mentioned glycinate and iminodiacetate substitution reactions, the a cetate groups of glycinate and iminodiacetate systems serve as the rea ction site for displacement of the chloride in the polysiloxane-immobi lized 3-chloropropyl system.