Reacción #81048

ord-6b2b8b24a609402ca8aa97326e39ae6e

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextracted 3×100 mL with ethyl acetate
  2. 2
    SecadoThe organic layer was dried (MgSO4)
  3. 3
    Filtraciónfiltered through silica gel
  4. 4
    Otroevaporated in vacuo
  5. 5
    Otroto give a crude solid which
  6. 6
    Otrowas recrystallized from cyclohexane/ethyl acetate

Procedimiento

6-(4-morpholinyl)-3-[3-(trifluoromethyl)phenyl]-1,5(6H)-pyridazindicarboxylic acid, diethyl ester (10.73 g, 0.024 mole) was refluxed in DMF (150 mL) for 30 min. The mixture was poured into water and extracted 3×100 mL with ethyl acetate. The organic layer was dried (MgSO4), filtered through silica gel, and evaporated in vacuo to give a crude solid which was recrystallized from cyclohexane/ethyl acetate to give 6-[3-(trifluoromethyl)phenyl]-4-pyridazinecarboxylic acid ethyl ester (3.34 g, 47% yield, Compound No. 1) as a brown solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05616789uspto-grants-1997_04