Sodium Azide → P,P-Diphenylphosphinic azide

Participants

Reaction Steps

Following the procedure of Baldwin and Washburn, J. Org. Chem., 30, 3860 (1965), 6.99 g (0.0297 mole) of diphenylphosphinyl chloride and 2.09 g (0.032 mole) of sodium azide were stirred in 40 ml of anhydrous acetone under a nitrogen atmosphere for 48 hours. The sodium chloride and unreacted sodium azide was removed by gravity filtration and the acetone solvent removed in vacuo. The crude diphenylphosphinic azide was analyzed for Cl content and in all cases only trace quantities (less than .1%) were found. The colorless diphenylphosphinic azide was purified by distillation to yield 6.31 g (87%) boiling at 138°-140° C./0.05 mm; literature value 137°-140° C./0.05 mm.

Provenance & Evidence