반응 #62406
ord-e7a4bb382256414d8ae1d3d86285d24e
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1세척The organic layer was successively washed with water and saturated brine
- 2건조dried over anhydrous magnesium sulfate
- 3기타the solvent was evaporated
- 4기타The residue was purified
- 5기타separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3)
실험 절차
To a solution of 22.5 g of 1-(5-bromo-6-fluoro-indazol-1-yl)ethanone in 250 mL of ethanol was added 20.0 mL of 5N sodium hydroxide aqueous solution at room temperature, and stirred at this temperature for 5 minutes. After neutralizing in 5N hydrochloric acid aqueous solution, the solution was diluted with ethyl acetate. The organic layer was successively washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3), to afford 16.7 g of the title compound as pale brown crystals.