반응 #80497

반응 방정식

N,N-dimethylformamide

2-chloro-4-trifluoromethyl phenol

potassium carbonate

5-(4-bromomethyl-3-chlorophenyl) 3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole

→

desired compound

수율 79.5%

3-(2-chloro-6-fluorophenyl)-5-[3-chloro-4(2-chloro-4-trifluoromethylphenoxymethyl)phenyl]-1-methyl-1H-1,2,4-triazole

수율 79.5%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONis added
2. 2
   workup.STIRRINGwhich is stirred at 120° C. for 1 hour
3. 3
   기타On completion of the reaction
4. 4
   온도the reaction solution is cooled to room temperature
5. 5
   추출extracted with toluene
6. 6
   세척The organic layer is washed with water
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   농축concentrated under reduced pressure
9. 9
   기타The concentrate is purified by silica gel column chromatography

실험 절차

To 30 ml of N,N-dimethylformamide are added 2-chloro-4-trifluoromethyl phenol (0.29 g) and potassium carbonate (0.25 g) and 5-(4-bromomethyl-3-chlorophenyl) 3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (0.60 g) is added thereto at room temperature with stirring, which is stirred at 120° C. for 1 hour. On completion of the reaction, the reaction solution is cooled to room temperature, poured into water and extracted with toluene. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography to give 0.61 g of desired compound (melting point: 113.0°-114.0° C.).

출처