Chlorodiphenylphosphine → Diphenylphosphine

Participants

Reaction Conditions

Reaction Steps

From Sodium Diphenylphosphide. To a suspension of sodium "sand" (4.6 g, 0.2 g atom) in a 100 ml of anhydrous dioxane heated at 65°-70° C. under nitrogen, a solution of diphenyl phosphorus chloride (22 g., 0.1 ml) in 50 ml of anhydrous dioxane is added during 1 hour. The solution is heated at reflux temperature (100° C) for 4 hours until all of the sodium is consumed. Then, after cooling to 10° C. 30 ml anhydrous ethanol is dropped in, followed by 25 ml of water to dissolve the sodium chloride. The organic layer is separated and the water is extracted with ether. The organic layers are dried and distilled in vacuum giving diphenylphosphine (14.14 g, 76 percent yield).

Provenance & Evidence