Reaktion #8170

ord-96385c6264c1424398d9348e12f7a5f7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under vacuum
  2. 2
    Waschenwashed with water (twice) and saturated sodium bicarbonate (once), and the organic layer
  3. 3
    Trocknendried over magnesium sulfate (MgSO4)
  4. 4
    FiltrationThe solid was filtered
  5. 5
    Sonstigethe solvents removed under vacuum
  6. 6
    SonstigeThe reaction product was purified over silica gel

Vorschrift

To 1-(4-nitrophenyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (0.5 g, 1.5 mmol) dissolved in methanol (4 mL) was added palladium on carbon and ammonium formate (0.428 g, 6.8 mmol). This mixture was stirred at room temperature overnight. The solvent was removed under vacuum, then the material was resuspended in chloroform, and washed with water (twice) and saturated sodium bicarbonate (once), and the organic layer dried over magnesium sulfate (MgSO4). The solid was filtered and the solvents removed under vacuum. The reaction product was purified over silica gel to yield the named product (m.p. 102° C.–103° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087634B2uspto-grants-2006_08