Reacción #89564

ord-f4c71742eea44a02906d33f912a0a436

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaat reflux for 18 h
  2. 2
    Concentraciónconcentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was carefully added a satd
  4. 4
    ExtracciónThe resulting mixture was extracted with CH2Cl2
  5. 5
    SecadoThe combined extracts were dried over anhydrous Na2SO4
  6. 6
    Filtraciónfiltered
  7. 7
    Concentraciónconcentrated under reduced pressure
  8. 8
    OtroThe residue obtained
  9. 9
    Otrowas dried under high vacuum

Procedimiento

A stirred solution of 6-bromo-2,3-difluorobenzoic acid and conc. H2SO4 in MeOH was heated at reflux for 18 h. The reaction mixture was cooled to rt and concentrated under reduced pressure. To the residue was carefully added a satd. aq. NaHCO3 solution. The resulting mixture was extracted with CH2Cl2. The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue obtained was dried under high vacuum to afford the title compound. ESI MS (M+H) 251.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09440982B2uspto-grants-2016_09