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The major product of the reaction of benzyl chloride with red phosphorus in the system concentrated aqueous KOH3dioxane3phase-transfer catalyst (43395oC, Ar) is tribenzylphosphine oxide (yield up to 61%). Under similar conditions, phosphorylation of benzyl chloride with white phosphorus occurs differently, yielding dibenzylphosphine oxide as major product. Conditions are found for preparative synthesis of dibenzylphosphine from phosphine and benzyl chloride in the system KOH3DMSO.