반응 #63137

반응 방정식

sodium carbonate

dichloroacetyl chloride

5-amino-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole

→

5-dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole

수율 93.5%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   여과filtered
2. 2
   세척washed in succession with water and saturated sodium chloride solution
3. 3
   건조The organic phase is dried over magnesium sulphate

실험 절차

15.3 g (0.145 mol) of anhydrous sodium carbonate and 4.76 ml (0.048 mol) of 98% strength dichloroacetyl chloride are added in succession, at 5° C. to 10° C., to 8.0 g (0.024 mol) of 5-amino-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole in 80 ml of dichloromethane. The mixture is stirred for 4 hours at 5° C.-10° C. and for 13 hours at room temperature. The mixture is diluted with 80 ml of dichloromethane, filtered, and washed in succession with water and saturated sodium chloride solution. The organic phase is dried over magnesium sulphate and freed from the solvent in vacuo. 10.0 g (93.5% of theory) of 5-dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 156° C.-161° C. are obtained.

출처