Tris (4-fluorophenyl)phosphine oxide could be used as a starting material to synthesize Tris(4-fluorophenyl)phosphine. Into the reactor were added 0.2 mmol of tris(4-fluorophenyl)phosphine oxide, 0.36 mmol of trifluoroacetic anhydride, and 1 ml of dioxane as a solvent. Stir at room temperature under a nitrogen atmosphere for 30 min; after the reaction, continue adding 0.2 mmol of sodium bicarbonate, 0.24 mmol of 15-Crown-5, and 1.2 mmol of sodium hydride under a nitrogen environment. Under 150 ℃, stir for 24 hours, stop the reaction, cool to room temperature, and distilled under reduced pressure to remove the solvent. The crude product is separated by column chromatography to obtain Tris(4-fluorophenyl)phosphine with a yield of 74%.