Acetone → Ruthenium bis bipyridyl dichloride

HRID 1081231ノート

反応式

HRID 1081231 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 9805343Ruthenium bis bipyridyl dichloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
15 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0b209bab7d8b4bb3aec4d4f3238c613a
出典データセット
uspto-grants-1996_12
特許番号
US05585279

反応ノート

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