Réaction #2275721

ord-6f347e622bc543babf746a6330d1acb8

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrereacted at 55° C. for 6 hours
  2. 2
    TempératureThe reaction solution was cooled
  3. 3
    Extractionthe reaction mixture was extracted twice with 10 mL ethyl acetate
  4. 4
    LavageThe ethyl acetate layer was washed with water
  5. 5
    Filtrationfiltered
  6. 6
    Concentrationconcentrated

Mode opératoire

0.17 g (0.4 mmol) of 5-amino-1-(2,6-dichloro-4-(trifluoromethyl) phenyl)-4-((trifluoromethyl) sulfinyl)-1H-pyrazol-3-carbonitrile, 0.01 g (0.03 mmol) of sodium tungstate.2H2O, and 0.07 g (0.6 mmol) of 30% aqueous hydrogen peroxide were dissolved in 1 mL acetic acid and reacted at 55° C. for 6 hours. The reaction solution was cooled, 10 mL water was added, and the reaction mixture was extracted twice with 10 mL ethyl acetate. The ethyl acetate layer was washed with water, then dehydrated over anhydrous magnesium sulfate, filtered and concentrated to give 0.2 g pale yellow crystal of 5-amino-1-(2,6-dichloro-4-(trifluoromethyl) phenyl)-4-((trifluoromethyl) sulfonyl)-1H-pyrazol-3-carbonitrile.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08323904B2uspto-grants-2012_12