1,4-Dibromo-2-nitrobenzene → 4,4'-Dibromo-2,2'-dinitro-1,1'-biphenyl
反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10]>CN(C=O)C.[Cu]>[Br:8][C:5]1[CH:6]=[CH:7][C:2]([C:2]2[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][C:3]=2[N+:9]([O-:11])=[O:10])=[C:3]([N+:9]([O-:11])=[O:10])[CH:4]=1参加物
4
反応条件
- 温度
- 25 °C
実験手順
The mixture of 1,4-dibromo-2-nitro-benzene (25 g, 89 mmol) and copper powder (12.5 g, 197 mmol) in DMF (150 ml) was heated at 137 C for 2 hours. The mixture was cooled to 25° C. and was quenched with water. The mixture was extracted with EtOAc (2×). The combined organic solution was washed with water and brine and was dried with Na2SO4. Concentration and purification by flash column chromatography (hexanes/EtOAc) gave 4,4′-dibromo-2,2′-dinitro-biphenyl (13.6 g).
後処理
- temperaturewas heated at 137 C for 2 hours
- customwas quenched with water
- extractionThe mixture was extracted with EtOAc (2×)
- washThe combined organic solution was washed with water and brine
- dry with materialwas dried with Na2SO4
- concentrationConcentration and purification by flash column chromatography (hexanes/EtOAc)
出典と根拠
- ORDレコード
- ord-60467a880edc4253afa85f3d2ca70f27
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08088368B2
反応ノート
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