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A variety of triphosphines [(Et 2 N) 2 P] 2 PR 4a–h, [( i Pr 2 N) 2 P] 2 PR 5a–e and [Ph 2 P] 2 PR 9e–g [R = Cy (a),  t Bu (b), Mes (c), Me 3 Si (d),  t BuMe 2 Si (e), ThexMe 2 Si (f),  i Pr 3 Si (g), Ad (h), H (i)] has been obtained by the reaction of the dilithiated primary phosphines RPH 2  la–h with 2 equiv. of the chlorophosphines (Et 2 N) 2 PCl 2, ( i Pr 2 N) 2 PCl 3 or Ph 2 PCl 8. Methanolysis of the trimethylsilyl substituted derivative [( i Pr 2 N) 2 P] 2 P(SiMe 3 ) 5d yields the hydrogen substituted triphosphine [( i Pr 2 N) 2 P] 2 PH 5i. The lithiated diphosphine ( i Pr 2 N) 2 P–P(SiMe 3 )Li 6 reacts with the chlorophosphine 2 to give the unsymmetrically substituted triphosphine ( i Pr 2 N) 2 P–P(SiMe 3 )–P(NEt 2 ) 2  7d. The compounds have been chracterized by their NMR and mass spectra. The structures of 4d and 9g have been determined by X-ray diffraction, representing the first structures of uncomplexed triphosphines.

zeitschrift für naturforschung b

Synthese amino- und silylsubstituierter Triphosphane – Struktur des 1.1.3.3-Tetrakis(di-iso-propylamino)-2-trimethylsilyl- und des 1.1.3.3-Tetraphenyl-2-tri-iso-propylsilyl-triphosphans / Synthesis of Amino- and Silyl-Substituted Triphosphines – Structure of 1,1,3,3-Tetrakis(di-iso-propylamino)-2-trimethylsilyl- and 1,1,3,3-Tetraphenyl-2-tri-iso-propylsilyl-triphosphine