반응 #1886582

ord-c800f94a85944a0097c741184ee73ad8

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the methanol was removed by evaporation under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in water (50 mL)
  3. 3
    추출extracted with EtOAc (3×25 mL)
  4. 4
    세척The combined extracts were washed with water and brine
  5. 5
    건조dried (MgSO4)
  6. 6
    기타evaporated

실험 절차

Ethyl 1-(4-bromophenyl)-5-cyclopropyl-pyrazole-4-carboxylate (Intermediate #31) (423 mg, 1.29 mmol) was dissolved in methanol (20 mL) and treated with 2M aqueous sodium hydroxide solution (3.23 mL, 6.46 mmol). The mixture was stirred at ambient temperature for 24 h and then the methanol was removed by evaporation under reduced pressure. The residue was dissolved in water (50 mL), acidified to pH4 with 2M HCl and extracted with EtOAc (3×25 mL). The combined extracts were washed with water and brine, dried (MgSO4) and evaporated to leave 1-(4-bromophenyl)-5-cyclopropyl-pyrazole-4-carboxylic acid a white solid. (343 mg, 87%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08344016B2uspto-grants-2013_01