반응 #504781

ord-60467a880edc4253afa85f3d2ca70f27

용매

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

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

DOI: 10.6084/m9.figshare.5104873.v1특허: US08088368B2uspto-grants-2012_01