Acetone → Ruthenium bis bipyridyl dichloride

HRID 1081231Notes

Reaction equation

HRID 1081231 reaction equation
O.O.O.[Ru:4](Cl)(Cl)[Cl:5].[N:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.[Cl-:20].[Li+].CC(C)=O>CN(C)C=O>[Cl-:5].[Cl-:20].[N:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.[N:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.[Ru+2:4]

Participants

6

Reactant 4

HCID 180AcetoneHCID 14742,2'-BipyridineHCID 433294Lithium ChlorideHCID 12090026Ruthenium chloride trihydrate

Product 1

HCID 9805343Ruthenium bis bipyridyl dichloride

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
15 °C

Procedure

A mixture of ruthenium trichloride trihydrate (2.5 g), 2,2' bipyridyl (3.0 g) and lithium chloride (5.0 g) was placed in 50 ml of DMF under nitrogen. This mixtrue was stirred and refluxed for 7 hours. The resulting purple/black solution was allowed to cool slowly to about 15° C. with continued stirring. 250 ml of acetone was then added and the flask stoppered under nigrogen. This solution was left at 0° C. for 24 hours. A black microcrystalline solid was recovered by filtration which was washed with water three times and diethyl ether three times.

Workup

  1. temperaturerefluxed for 7 hours
  2. filtrationA black microcrystalline solid was recovered by filtration which
  3. washwas washed with water three times and diethyl ether three times

Sources & evidence

ORD record
ord-0b209bab7d8b4bb3aec4d4f3238c613a
Source dataset
uspto-grants-1996_12
Patent number
US05585279

Reaction notes

Loading…