Reaction #2275721

Reaction equation

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

hydrogen peroxide

water

→

pale yellow crystal

Yield 110.3%

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

Yield 110.3%

Solvents

acetic acid

Conditions

Workup

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

Procedure

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