Reaktion #67276

ord-654553996de24bb3b9c3cb617d7d71f5

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigebrought to ambient temperature
  2. 2
    Sonstigethe phases were separated
  3. 3
    Extraktionthe water phase extracted with EtOAc
  4. 4
    WaschenThe combined organic phases were washed with brine
  5. 5
    Trocknendried (Na2SO4)
  6. 6
    Sonstigeevaporated to dryness

Vorschrift

AlCl3 (5.0 g, 38 mmol) was added in portions to 4-bromo-2-fluorophenyl acetate (5.8 g, 25 mmol). The mixture was heated at 150° C. for 3 h and then brought to ambient temperature. Water (ice-cold) was slowly added and then EtOAc. The resulting mixture was vigorously stirred and then the phases were separated and the water phase extracted with EtOAc. The combined organic phases were washed with brine, dried (Na2SO4) and evaporated to dryness to give the title compound (5.3 g). MS m/z (rel. intensity, 70 eV) 233 (M+, 55), 232 (M+, 56), 218 (98), 217 (bp), 161 (10).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524766B2uspto-grants-2013_09