Реакция #40718

ord-4325811208714cde96d7855dd97c1686

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураWhen cooled
  2. 2
    Экстракцияthe aqueous layer was extracted with EtOAc (2×15 mL)
  3. 3
    ПромывкаThe combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
  4. 4
    Сушкаdried with NaSO4
  5. 5
    Фильтрацияfiltered
  6. 6
    ДругоеAfter evaporation of the solvent
  7. 7
    Другоеlight brown solids were obtained (0.15 g, 62%)
  8. 8
    ДругоеThe compound was used in the next synthetic step without further purification

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07728016B2uspto-grants-2010_06