Triphenylphosphine → HCID 11041943, compound

HRID 1249608Notes

Reaction equation

HRID 1249608 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([P:9]([Cl:12])([Cl:11])=O)[CH:5]=[CH:6][C:7]=1[CH3:8].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>>[Cl:11][P:9]([Cl:12])[C:4]1[CH:5]=[CH:6][C:7]([CH3:8])=[C:2]([CH3:1])[CH:3]=1

Participants

3

Reactant 2

HCID 11776TriphenylphosphineHCID 54455750HCID 54455750, compound

Product 1

HCID 11041943HCID 11041943, compoundYield 92%

Procedure

121 g (0.52 mole) of 3,4-dimethylphenylphosphonic acid dichloride and 283 g (1.08 moles) of triphenylphosphane were stirred for 11 hours at 200° C. under an atmosphere of nitrogen. Distillation was then carried out until an internal temperature of 170° C. at 0.067 kPa was reached. This gave 120 g, containing 45% of dichloro-3,4dimethylphenylphosphane and 48% of 3,4-dimethylphenylphosphonic acid dichloride. This corresponds to a yield of approx. 92% of theory at a conversion of 52.2%. Fractional distillation of the crude distillate gave pure dichloro-3,4-dimethylphenylphosphane, boiling point: 107° C./0.44 kPa.

Workup

  1. distillationDistillation
  2. customwas then carried out until an internal temperature of 170° C. at 0.067 kPa
  3. additionThis gave 120 g, containing 45% of dichloro-3,4dimethylphenylphosphane and 48% of 3,4-dimethylphenylphosphonic acid dichloride
  4. distillationFractional distillation of the crude distillate

Sources & evidence

ORD record
ord-93b86e26700347658bf94d5b45bf1cbf
Source dataset
uspto-grants-1986_12
Patent number
US04632995

Reaction notes

Loading…