Phosphine, tris(4-methylphenyl)- → HCID 10855191, compound

HRID 2058569Notes

Reaction equation

HRID 2058569 reaction equation
[C:1]1([CH3:22])[CH:6]=[CH:5][C:4]([P:7]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)[C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.O.[Ru:24](Cl)([Cl:26])[Cl:25]>CO>[Ru:24]([Cl:26])[Cl:25].[C:18]1([CH3:21])[CH:19]=[CH:20][C:15]([P:7]([C:8]2[CH:9]=[CH:10][C:11]([CH3:14])=[CH:12][CH:13]=2)[C:4]2[CH:5]=[CH:6][C:1]([CH3:22])=[CH:2][CH:3]=2)=[CH:16][CH:17]=1.[C:18]1([CH3:21])[CH:19]=[CH:20][C:15]([P:7]([C:8]2[CH:9]=[CH:10][C:11]([CH3:14])=[CH:12][CH:13]=2)[C:4]2[CH:5]=[CH:6][C:1]([CH3:22])=[CH:2][CH:3]=2)=[CH:16][CH:17]=1.[C:18]1([CH3:21])[CH:19]=[CH:20][C:15]([P:7]([C:8]2[CH:9]=[CH:10][C:11]([CH3:14])=[CH:12][CH:13]=2)[C:4]2[CH:5]=[CH:6][C:1]([CH3:22])=[CH:2][CH:3]=2)=[CH:16][CH:17]=1

Participants

4

Reactant 2

HCID 13956Phosphine, tris(4-methylphenyl)-HCID 6093376Ruthenium trichloride hydrate

Product 1

HCID 10855191HCID 10855191, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Using the procedure of Example 1, 50 mls. of methanol, 6.0 grams of tri-paratolylphosphine and 1.0 gram of ruthenium trichloride hydrate are stirred and heated at reflux under nitrogen for 24 hours to form tris(tri-paratolylphosphine) ruthenium dichloride as an insoluble powder which is recovered by filtration (4.2 grams). A portion of this powder (0.5 gram) is dissolved in a mixture containing 50 mls. of methanol and 0.5 gram of anhydrous sodium acetate. The resulting mixture is heated with stirring at reflux temperature under nitrogen for 5 hours to form yellow solids (0.21 gram) which are identified as the desired hydridoacetato ruthenium tris(tri-paratolylphosphine).

Workup

  1. temperatureheated
  2. temperatureat reflux under nitrogen for 24 hours

Sources & evidence

ORD record
ord-838d7fd977524ea1aaae308c12ae10b6
Source dataset
uspto-grants-1982_03
Patent number
US04317946

Reaction notes

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