Reaktion #169410

ord-2ca0929cdc1943a5bb7da6b308a0cd5c

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was evaporated in vacuo
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in water (50 mL)
  3. 3
    Waschenthen washed with EtOAc (100 mL)
  4. 4
    Extraktionextracted with 10% IPA in DCM (4×100 mL)
  5. 5
    TrocknenThe combined organic phases were dried over sodium sulphate
  6. 6
    Sonstigeevaporated in vacuo

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846698B2uspto-grants-2014_09