Reaktion #51850

ord-baeea72672b647a4baeb6e9fbd6b854b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeexcess acetic acid evaporated off
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in hot ethyl acetate (25 ml)
  3. 3
    Filtrationbenzene (25 ml) and filtered
  4. 4
    TemperaturAfter cooling to room temperature
  5. 5
    Filtrationthe mixture was filtered
  6. 6
    Sonstigethe residue recrystallized from 50% aqueous ethanol (20 ml)
  7. 7
    Sonstigeto give 0.58 g (53%)

Vorschrift

A mixture of 1,2-diphenyl-4-(4-methylphenyl)-3,5-pyrazolidinedione (1.10 g; 3.2 =mol), 35% H2O2 (0.47 ml; 5.5 mmol), and acetic acid (40 ml) was stirred 16 days at room temperature. Sodium metabisulfite (1.0 g) was added and excess acetic acid evaporated off. The residue was dissolved in hot ethyl acetate (25 ml) and benzene (25 ml) and filtered. After cooling to room temperature, the mixture was filtered and the residue recrystallized from 50% aqueous ethanol (20 ml) to give 0.58 g (53%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06852749B1uspto-grants-2005_02