반응 #167033

반응 방정식

1,4-dibromo-2-nitro-benzene

→

4,4′-dibromo-2,2′-dinitro-biphenyl

수율 76.0%

용매

DMF

반응 조건

후처리

1. 1
   온도was heated at 137 C for 2 hours
2. 2
   기타was quenched with water
3. 3
   추출The mixture was extracted with EtOAc (2×)
4. 4
   세척The combined organic solution was washed with water and brine
5. 5
   건조was dried with Na2SO4
6. 6
   농축Concentration and purification by flash column chromatography (hexanes/EtOAc)

실험 절차

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).

출처