反応 #159087

反応方程式

1,4-dibromo-2-nitro-benzene

→

4,4′-dibromo-2,2′-dinitro-biphenyl

収率 76.0%

溶媒

DMF

反応条件

後処理

1. 1
   温度was heated at 137 C for 2 hours
2. 2
   その他was quenched with water
3. 3
   抽出The mixture was extracted with EtOAc (2×)
4. 4
   洗浄The combined organic solution was washed with water and brine
5. 5
   乾燥was dried with Na2SO4
6. 6
   濃縮Concentration and purification by flash column chromatography (hexanes/EtOAc)

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).

出典