Phosphorus trichloride → HCID 53977937, compound
Reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([P:9]([Cl:11])Cl)[CH:5]=[CH:6][C:7]=1[CH3:8].P(Cl)(Cl)Cl>[Cl-].[Zn+2].[Cl-]>[CH3:1][C:2]1[CH:3]=[C:4]([P:9]([Cl:11])[C:4]2[CH:5]=[CH:6][C:7]([CH3:8])=[C:2]([CH3:1])[CH:3]=2)[CH:5]=[CH:6][C:7]=1[CH3:8]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 120 °C
Procedure
A mixture of 3,4-dimethylphenyl phosphonous dichloride (37.6 g) and freshly prepared anhydrous zinc chloride (1.96 g) was heated at 280°-320° C. in a distillation apparatus which incorporated a heated fractionating head, maintained at 120° C. The reaction was carried out under a reduced pressure of approximately 200 mmHg for a period of 5 hours. Phosphorus trichloride (12.4 g) was evolved during the reaction and was trapped out using liquid nitrogen. The reaction mixture was then fractionally distilled under reduced pressure by increasing the vacuum. Unreacted starting material was distilled off, as a colourless liquid, at 70°-125° C. at 0.05 mmHg pressure. Product bis(3,4-dimethylphenyl) phosphinous monochloride, was then distilled, as a colourless liquid, at 130°-155° C. and a pressure of 0.05 mmHg. The product weighed 12.5 g, equivalent to a yield of 56.7% based on a conversion of 87.8%. It has a melting point of 36°-38° C.
Workup
- temperaturewas heated at 280°-320° C. in a distillation apparatus which incorporated a heated fractionating head
- distillationThe reaction mixture was then fractionally distilled under reduced pressure
- temperatureby increasing the vacuum
- distillationwas distilled off, as a colourless liquid, at 70°-125° C. at 0.05 mmHg pressure
- distillationProduct bis(3,4-dimethylphenyl) phosphinous monochloride, was then distilled, as a colourless liquid, at 130°-155° C.
Sources & evidence
- ORD record
- ord-6d96f3cb17504c2eb85d303849b55693
- Source dataset
- uspto-grants-1980_12
- Patent number
- US04238422
Reaction notes
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