Diphenylphosphine oxide → Diphenylphosphine

HRID 265816Notes

Reaction equation

HRID 265816 reaction equation
[C:1]1([PH:7](=O)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Al+3].[Cl-].[Cl-]>>[C:8]1([PH:7][C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Participants

3

Reactant 2

HCID 254003Diphenylphosphine oxideHCID 6451240Aluminum(III) Chloride

Product 1

HCID 70017DiphenylphosphineYield 90%

Conditions

Temperature
157 °C

Procedure

101 g (0.5 mol) of diphenylphosphine oxide and 0.5 g of aluminum chloride are mixed and heated to 157° C., the pressure being reduced simultaneously (12 mbar). Diphenylphosphine distills off through a descending condenser at a transition temperature of 144° C. The internal temperature is finally raised to 183° C. 42 g of diphenylphosphine are obtained with a purity of 99% according to 31P NMR. That corresponds to a yield of 90% of theory.

Workup

  1. distillationDiphenylphosphine distills off through a descending condenser at a transition temperature of 144° C
  2. temperatureThe internal temperature is finally raised to 183° C

Sources & evidence

ORD record
ord-087d95bcbbb5410b8f1e28333eb47f84
Source dataset
uspto-grants-1997_07
Patent number
US05648549

Reaction notes

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