반응 #40719

ord-71fa31f77a6743d998658e65f9b69f56

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After evaporation of the solvent, EtOAc (20 mL)
  2. 2
    workup.ADDITIONwas added
  3. 3
    세척The organic layer was then washed with sat. NaHCO3 (2×10 mL) and brine (20 mL)
  4. 4
    건조dried with NaSO4
  5. 5
    여과filtered
  6. 6
    기타After evaporation of the solvent
  7. 7
    기타light brown semi-solids (93 mg, 57%) were obtained
  8. 8
    기타purified by prep

실험 절차

1-(2,4-Dihydroxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid (0.15 g, 0.48 mmol) was refluxed in EtOH (20 mL) in the presence of 5 drops of concentrated H2SO4 for 3 hours. After evaporation of the solvent, EtOAc (20 mL) was added. The organic layer was then washed with sat. NaHCO3 (2×10 mL) and brine (20 mL), dried with NaSO4 and filtered. After evaporation of the solvent, light brown semi-solids (93 mg, 57%) were obtained and purified by prep. TLC (Rf=0.73, EtOAc).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728016B2uspto-grants-2010_06