Tetraphenyldiphosphine, from the initial preparation, was added to 25 ml of toluene containing sufficient sulfur for complete reaction.The mixture was heated to with stirring, under an inert atmosphere for 6 hr. The hot toluene solution was then filtered and evaporated. This reaction resulted in essentially 100% conversion based on the initial quantity of tetraphenyldiphosphine.The white crystals obtained from this reaction were recrystallized from chloroform-methanol and vacuum dried. The infrared spec-trum83 was identical with that reported for tetraphenyldiphosphine disulfide. The mass spectrum was consistent, exhibiting a peak at 434, attributable to the parent ion [(C6H5)2P(S)P(S)(C6H5)2, mol wt 434], Diphenylphosphinic Anhydride, (CGH5)2P(0)0P(0)(CeH:)2. Tetraphenyldiphosphine, 0.22 g (0.6 mmol) from the initial preparation, was added to 15 ml of toluene containing a small amount of diphenylchlorophosphine (0.05 g). Dry oxygen in excess was introduced into the solution at room temperature, and the reaction continued until oxygen take-up ceased. The toluene solution was then filtered through decolorizing charcoal, concentrated by evaporation under vacuum, and allowed to stand at room temperature.The crystals which formed on standing were washed repeatedly with dry, cold heptane or ether and dried under vacuum at room temperature. The material was then recrystallized several times from toluene. In this preparation as in those above, the presence of moisture led to the formation of diphenylphosphinic acid, which was removed by washing with 1 % aqueous potassium hydroxide as described previously.Diphenylphosphinic anhydride melted at 144-145°, lit.10 142-143°. Its infrared spectrum contained a band at 1236 cm-1 assigned to the P=Ozl stretching frequency and a band at 960 cm-1 assigned to the P-O-P22 linkage.Mass spectral data showed a parent ion peak corresponding to a mass of 418 [(C6H6)2P(0)0P(0)(CeH6)2; mol wt 418], and a fragmentation pattern consistent with that of diphenylphosphinic anhydride.