Reacción #167033

ord-ac6bbfcd40564d969d7f01b1eb90fa62

Disolventes

Condiciones de reacción

Temperatura
25°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated at 137 C for 2 hours
  2. 2
    Otrowas quenched with water
  3. 3
    ExtracciónThe mixture was extracted with EtOAc (2×)
  4. 4
    LavadoThe combined organic solution was washed with water and brine
  5. 5
    Secadowas dried with Na2SO4
  6. 6
    ConcentraciónConcentration and purification by flash column chromatography (hexanes/EtOAc)

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08841278B2uspto-grants-2014_09