Reacción #62406

ord-e7a4bb382256414d8ae1d3d86285d24e

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    LavadoThe organic layer was successively washed with water and saturated brine
  2. 2
    Secadodried over anhydrous magnesium sulfate
  3. 3
    Otrothe solvent was evaporated
  4. 4
    OtroThe residue was purified
  5. 5
    Otroseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07429609B2uspto-grants-2008_09