반응 #2275721

반응 방정식

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

hydrogen peroxide

water

→

pale yellow crystal

수율 110.3%

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

수율 110.3%

용매

acetic acid

반응 조건

후처리

1. 1
   기타reacted at 55° C. for 6 hours
2. 2
   온도The reaction solution was cooled
3. 3
   추출the reaction mixture was extracted twice with 10 mL ethyl acetate
4. 4
   세척The ethyl acetate layer was washed with water
5. 5
   여과filtered
6. 6
   농축concentrated

실험 절차

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.

출처