Reacción #45575

ord-9aa13dd326e54abfb0181b08fd8f4200

Disolventes

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter cooling
  2. 2
    Otromethanol was evaporated away under reduced pressure
  3. 3
    Extracciónfollowed by extraction with ethyl acetate
  4. 4
    Lavadowashing with saturated brine
  5. 5
    Secadodrying on anhydrous magnesium sulfate
  6. 6
    Concentraciónthe solvent was concentrated under reduced pressure
  7. 7
    Otroto obtain a pale brown residue
  8. 8
    OtroThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1)

Procedimiento

Aqueous potassium carbonate solution (1.25 ml) [potassium carbonate (15 g) was dissolved in water (100 ml)] and methanol (1.25 ml) were added to N-(2-bromo-5-cyano-3-methoxy-6-methylbiphenyl-4-yl)2,2,2-trifluoroacetamide (I-38) (133 mg, 0.322 mmol), followed by stirring overnight at 70° C. After cooling, methanol was evaporated away under reduced pressure, followed by extraction with ethyl acetate, washing with saturated brine and drying on anhydrous magnesium sulfate, the solvent was concentrated under reduced pressure to obtain a pale brown residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1) to obtain the entitled compound (95 mg, 94%) as a colorless solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07737166B2uspto-grants-2010_06