Reacción #169410

ord-2ca0929cdc1943a5bb7da6b308a0cd5c

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe mixture was evaporated in vacuo
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in water (50 mL)
  3. 3
    Lavadothen washed with EtOAc (100 mL)
  4. 4
    Extracciónextracted with 10% IPA in DCM (4×100 mL)
  5. 5
    SecadoThe combined organic phases were dried over sodium sulphate
  6. 6
    Otroevaporated in vacuo

Procedimiento

Aqueous sodium hydroxide (150 mL of a 1 M solution) was added to [1-isopropyl-5-(trifluoromethyl)-1H-pyrazol-4-yl]acetonitrile (Preparation 184, 6.2 g, 28.6 mmol) in EtOH (150 mL) and the mixture was heated at 60° C. for 16 hours. The mixture was evaporated in vacuo and the residue was dissolved in water (50 mL) then washed with EtOAc (100 mL). The aqueous phase was acidified to pH 5 using 1N HCl and extracted with 10% IPA in DCM (4×100 mL). The combined organic phases were dried over sodium sulphate and evaporated in vacuo to afford the title compound as a white solid in 75% yield, 5.0 g.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08846698B2uspto-grants-2014_09