반응 #1584540

ord-165416b5939f40028c1703667155e057

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the mixture was extracted with ethyl acetate
  2. 2
    세척The organic layer was washed with saturated brine
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타The obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate)

실험 절차

To a solution of 5-bromo-3-methyl-1H-indazole (8.44 g) in ethyl acetate (100 ml) was added dropwise triethyloxonium tetrafluoroborate (1 M dichloromethane solution, 60 ml) at room temperature, and the mixture was stirred at the same temperature overnight. To the reaction mixture was added a 1 M aqueous sodium hydroxide solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate) to give the title compound (1.3 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09199963B2uspto-grants-2015_12