Triphenylphosphine → Dichlorotris(triphenylphosphine)ruthenium

HRID 2058567Notes

Reaction equation

[C:1]1([P:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[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.O.[Ru:21](Cl)([Cl:23])[Cl:22]>CO>[Ru:21]([Cl:23])[Cl:22].[C:14]1([P:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1.[C:14]1([P:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1.[C:14]1([P:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

Participants

Conditions

Temperature: 75 °C

Procedure

To a 100 cc glass flask is added 50 mls. of methanol, 5.0 gram of triphenylphosphine and 1.0 gram of ruthenium trichloride hydrate. The resulting mixture is stirred and heated by means of an oil bath under an atmosphere of nitrogen to a temperature of 75° C. and maintained at that temperature for 6 hours. Tris(triphenylphosphine) ruthenium dichloride is formed as a brown insoluble powder, which is recovered by filtration (3.9 gram). 1.0 Gram of this powder is dissolved in a mixture containing 150 mls. of methanol and 1.5 grams of sodium acetate trihydrate. The mixture is stirred and then heated under N2 by means of an oil bath to a temperature of 75° C. which is maintained for a period of 4 hours. This results in formation of a yellow precipitate, which is recovered by filtration and is identified as the desired hydridoacetato tris(triphenylphosphine) ruthenium (0.8 gram).

Workup

additionTo a 100 cc glass flask is added 50 mls
temperaturemaintained at that temperature for 6 hours

Sources & evidence

ORD record: ord-f99f5ac89ae14f81b08de671f3c55fdf
Source dataset: uspto-grants-1982_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04317946

Reaction notes

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