Reacción #40718

ord-4325811208714cde96d7855dd97c1686

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaWhen cooled
  2. 2
    Extracciónthe aqueous layer was extracted with EtOAc (2×15 mL)
  3. 3
    LavadoThe combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
  4. 4
    Secadodried with NaSO4
  5. 5
    Filtraciónfiltered
  6. 6
    OtroAfter evaporation of the solvent
  7. 7
    Otrolight brown solids were obtained (0.15 g, 62%)
  8. 8
    OtroThe compound was used in the next synthetic step without further purification

Procedimiento

1-(5-Chloro-2,4-dimethoxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid (0.29 g, 0.77 mmol) was refluxed in a mixture of hydroiodic acid (5 mL), acetic acid (1 mL) and acetic anhydride (0.5 mL) for 16 hours. When cooled, water (20 mL) was added and the aqueous layer was extracted with EtOAc (2×15 mL). The combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL), dried with NaSO4 and filtered. After evaporation of the solvent, light brown solids were obtained (0.15 g, 62%). The compound was used in the next synthetic step without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07728016B2uspto-grants-2010_06