Triphenylphosphine → Phenyl phosphorus dichloride

HRID 1249606Notes

Reaction equation

[C:1]1([P:7]([Cl:10])([Cl:9])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>>[Cl:9][P:7]([Cl:10])[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

Reactant 2

HCID 11776Triphenylphosphine

HCID 69990Phenylphosphonic dichloride

Product 1

HCID 12573Phenyl phosphorus dichlorideYield 91%

Procedure

50 g (0.256 mole) of phenylphosphonic acid dichloride and 40 g (0.153 mole) of triphenylphosphane were stirred for 12 hours at 230° C. under an atomosphere of nitrogen. Distillation was then carried out at 0.1 kPa until an internal temperature of 200° C. was reached. The distillate obtained was then fractionated using a silvered-jacketed column, 70 cm long, packed with Raschig rings. 25 g of dichlorophenylphosphane were obtained, as well as unreacted phenylphosphonic acid dichloride. This corresponds to a yield of 91% of theory, based on triphenylphosphane employed.

Workup

distillationDistillation
customwas then carried out at 0.1 kPa until an internal temperature of 200° C.
customThe distillate obtained

Sources & evidence

ORD record: ord-d1aeafc81edb4ee685d1a40828899745
Source dataset: uspto-grants-1986_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04632995

Reaction notes

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