THE SYNTHESIS AND CHARACTERIZATION OF A BARIUM SILYL-PHOSPHIDE BY A LOW-TEMPERATURE ROUTE

The reaction of tetramethylsilane and sodium hydride in a mixed solvent of THF and HMPA (2:1 by volume), at reflux for 40 h, followed by the addition of PCl3 yielded (Me3Si)3P (1) in excellent yield by a simple, non-hazardous and facile route. This phosphine was readily converted into the known phosphide (Me3Si)2PH (2) by controlled hydrolysis. Reaction of this ligand with barium granules in a mixed liquid ammonia-THF solvent system at -40-degrees-C yielded the first barium silylphosphide, [Ba(P{SiMe3}2)2(THF)2]n (3). which was characterized by IR, H-1, C-13 and Si-29 NMR spectroscopy.