Hydrochloric Acid → Bis(tri-o-tolylphosphine)palladium(II) Dichloride

HRID 1277543Notes

Reaction equation

HRID 1277543 reaction equation
[Pd:1]([Cl:3])[Cl:2].Cl.[C:5]1([CH3:26])[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[P:11]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[CH3:25])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:18]>C(O)C>[Pd:1]([Cl:3])[Cl:2].[C:5]1([CH3:26])[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[P:11]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[CH3:25])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:18].[C:5]1([CH3:26])[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[P:11]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[CH3:25])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:18]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 24290Palladium ChlorideHCID 80271Tri-o-tolylphosphine

Product 1

HCID 10876480Bis(tri-o-tolylphosphine)palladium(II) DichlorideYield 99.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Into a 1-l round flask 10.65 g (0.06 mole) of palladium chloride, 300 ml ofwater and 30 ml of concentrated hydrochloric acid were introduced, and after dissolving the solid material uniformly with agitation, 36.5 g (0.12mole) of tri(ortho-tolyl)phosphine were added to the mixed solution, and after further introducing 300 ml of ethanol, the mixed solution was refluxed under heating for 2.5 hours. After cooling, the reaction mixture was filtered and the filtrate was washed with ethanol and then dried, obtaining 41.2 g of yellow bis[tri(ortho-tolyl)phosphine] palladium chloride, ##STR8##(decomposition temperature: 272°-278° C.) in a yield of 99.9%.

Workup

  1. additionwere added to the mixed solution
  2. temperaturethe mixed solution was refluxed
  3. temperatureunder heating for 2.5 hours
  4. temperatureAfter cooling
  5. filtrationthe reaction mixture was filtered
  6. washthe filtrate was washed with ethanol
  7. customdried

Sources & evidence

ORD record
ord-d93be5aa85444ce1a5b7c40e0577164c
Source dataset
uspto-grants-1981_07
Patent number
US04277633

Reaction notes

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