Reaktion #5249

ord-235b5db98cd94164b1a080341731bb8b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture has been refluxed for 3 hours
  2. 2
    SonstigeAfterwards, almost all of the solvent has been evaporated
  3. 3
    workup.ADDITIONwater and ice have been added to the residue
  4. 4
    Filtrationthe precipitate has been collected by filtration

Vorschrift

Compound (H) (5 g; 17.5 mmols) has been dissolved in warm toluene (25 ml). To this solution, an equimolar amount of potassium tert. butylate has been added and the reaction mixture has been refluxed for 3 hours. Afterwards, almost all of the solvent has been evaporated; water and ice have been added to the residue and the precipitate has been collected by filtration. The thus obtained crude (J) has been recrystallized from ethanol (3.7 g; yield, 88%); m.p. 130°-131° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05243056uspto-grants-1993_09