Reaktion #2275721

Reaktionsgleichung

5-amino-1-(2,6-dichloro-4-(trifluoromethyl) phenyl)-4-((trifluoromethyl) sulfinyl)-1H-pyrazol-3-carbonitrile

hydrogen peroxide

water

→

pale yellow crystal

Ausbeute 110.3%

5-amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-((trifluoromethyl)sulfonyl)-1H-pyrazol-3-carbonitrile

Ausbeute 110.3%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigereacted at 55° C. for 6 hours
2. 2
   TemperaturThe reaction solution was cooled
3. 3
   Extraktionthe reaction mixture was extracted twice with 10 mL ethyl acetate
4. 4
   WaschenThe ethyl acetate layer was washed with water
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated

Vorschrift

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.

Quelle