Neuartige basische Liganden fuer die homogenkatalytische Methanolcarbonylierung XVIII. Darstellung und Charakterisierung von an Kieselgel fixierten Ether-Phosphanen mit Spacern von drei und sechs Kohlenstoffatomen

Article abstract of DOI:10.1016/0022-328X(88)89009-0

The silylalkyl(ether-phosphanes) XnMe3-nSi(CH2)m+2P(Ph)D (3a, b, e, 4a, b, e, 5a) are obtained by photochemically induced addition of the secondary phosphanes HP(Ph)D to the olefinic double bond of the ω-alkenylchloro- and ω-alkenylmethoxysilanes XnMe3-nSi(CH2)mCH=CH2.The corresponding silylalkyl(ether-phosphanes) 3c, d, 4c, d and 5c are obtained from the reaction of the chloropropylmethoxysilanes XnMe3-nSi(CH2)m+2Cl (2c, d) with HP(Ph)D in the presence of NaH.The ligands 3a, b, d, e, 4a, b, d, e and 5a can be attached to silica gel.For HCl cleavage lutidine is used as an auxiliary base in the case of the chlorine-containing silylalkyl(ether-phosphanes) 3a, b, 4a, b, 5a. 13C, 29Si, and 31P CP-MAS NMR spectra indicate succesful heterogenization, thus giving insight into the nature of the bonding of the ligands with the surface of the silica gel.