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The synthesis of the trimethylsilyl derivatives of the PH-functional methylenebisphosphanes, R 2-n (Me 3  Si) n P-CH 2  -PR(SiMe 3 ) (R = Me, iPr, tBu, Ph, 2.4.6-Me 3 C 6 H 2  ; n = 0.1) is reported. In the Li-phosphides R 2-n Li n P - CH 2  - PLiR used as reactive intermediates, a monomer-oligomer association equilibrium causes a rapid Li-exchange as indicated by the solvent and temperature dependent  31 P{ 1 H} and  7 Li NMR spectrum of (iPr) 2  P-CH 2  -P(iPr)Li in various solvents (Et 2 O, THF and MTHF) in the temperature range from 30 to -110 °C. For the syntheses of the Me-and Ph-substituted PH-functional methylenebisphosphanes R 2 P-CH 2  -PRH and RHP-CH 2  -PRH (R = Me, Ph) the chlorophosphane CKP -CH 2  -PCl 2  is used as a starting material. Bifunctional substituents (Ph -N̍-N̍ -Ph and Me -N̍-CO-N̍-Me) are employed for the first time as protecting groups to block one or two PCl-functions in Cl 2 P-CH 2 -PCI 2 ,. Cleavage of the PN-bonds in the five membered ring systems(R = Me, Ph) with HCl affords the P-substituted methylenebis-chlorophosphanes RClP-CH 2  - PClR in satisfactory yields.

zeitschrift für naturforschung b

Lineare Oligophosphaalkane, XX [1]: Alkalimetall-und Trimethylsilylderivate PH-funktioneller Methylenbisphosphane / Linear Oligophosphaalkanes, XX [1]: Alkali Metal and Trimethylsilyl Derivatives of PH-Functional Methylenebisphosphanes