Hydrochloric Acid → Diphenylphosphine

Participants

Reaction Steps

20×10-3 cm3 of 1,2-dibromoethane was added dropwise in a nitrogen gas atmosphere to a suspension of 461 mg (7.05 mg-atoms) of zinc (powder) in 10 cm3 of tetrahydrofuran, the mixture was heated to reflux for about 2 minutes and cooled to room temperature, 30×10-3 cm3 of chlorotrimethylsilane was added and the mixture was stirred for about 2 minutes to prepare an activated zinc. Subsequently, 1.04 g (4.71 mmol) of chlorodiphenylphosphine was added dropwise and the mixture was stirred at room temperature. To the reaction mixture was added dropwise 10 cm3 (10 mmol) of 1 mol·dm-3 hydrochloric acid and then 10 cm3 of toluene. The mixture was stirred, the aqueous layer and the toluene layer were separated off, the toluene layer was determined by gas chromatography, giving diphenylphosphine in 84% yield.

Provenance & Evidence