반응 #80521

반응 방정식

N,N-dimethylformamide

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

potassium acetate

→

desired compound

수율 51.1%

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

수율 51.1%

용매

water

반응 조건

후처리

1. 1
   온도The reaction mixture is cooled to room temperature
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The organic layer is washed with water
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated under reduced pressure
6. 6
   기타The concentrate is purified by silica gel column chromatography
7. 7
   workup.ADDITIONusing mixed solvent of hexaneethyl acetate as eluent

실험 절차

To N,N-dimethylformamide (200 ml) are added 5-(4-bromomethyl-3-chlorophenyl)-3(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (24.3 g) and potassium acetate (29.0 g), which are stirred at 130° C. for 3 hours. The reaction mixture is cooled to room temperature, poured into water and extracted with ethyl acetate. 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 using mixed solvent of hexaneethyl acetate as eluent to give 11.8 g of desired compound.

출처