Réaction #51850

ord-baeea72672b647a4baeb6e9fbd6b854b

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autreexcess 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
    TempératureAfter cooling to room temperature
  5. 5
    Filtrationthe mixture was filtered
  6. 6
    Autrethe residue recrystallized from 50% aqueous ethanol (20 ml)
  7. 7
    Autreto give 0.58 g (53%)

Mode opératoire

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%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06852749B1uspto-grants-2005_02