Tetraphenyl-l, 2,3-triphospholenyl Hexachlorostannate

The corresponding tetrachloroaluminate can be obtained from [(PhjP)2P] [AICI4] (see Section A) and bis(diphenylphosphino)ethane.  

2-dimethoxymethane, with some benzophenone (2.0 g) added, is heated at reflux with excess sodium (N2 atmosphere, copper condenser) until the blue color persists and is then distilled. Dichloromethane is dried as in Section A. Phosphorus trichloride is freshly distilled under normal pressure. 

Hexamethylphosphorous triamide is used as commercially available, for larger quantities it is economically prepared from PCI, and Me2NH. All equipment is oven-dried, evacuated, and flushed with Nj or Ar. 

The compound [Me2N)3P]2P [BPh4] forms colorless crystals, mp 161 °C, soluble in dichloromethane and benzonitrile, less soluble in tetrahydrofuran (THF) and chlorobenzene. P H NMR A2B, 5 + 85, —194, 

Submitted by WAN AHMAD KAMIL and JEAN NE M. SHREEVE Checked by ROBERT R. HOLMES and KUMARA SWAMY  

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