反应 #62406

ord-e7a4bb382256414d8ae1d3d86285d24e

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤The organic layer was successively washed with water and saturated brine
  2. 2
    干燥dried over anhydrous magnesium sulfate
  3. 3
    其他the solvent was evaporated
  4. 4
    其他The residue was purified
  5. 5
    其他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07429609B2uspto-grants-2008_09