반응 #158313

반응 방정식

1-(4-bromo-2-fluorophenyl)-3-methyl-1H-1,2,4-triazole

potassium carbonate

ethanol

DMF

→

title compound

3-fluoro-4-(3-methyl-1H-1,2,4-triazol-1-yl)benzonitrile

용매

water

brine

반응 조건

후처리

1. 1
   온도to cool to room temperature
2. 2
   추출the mixture was extracted with ethyl acetate
3. 3
   세척The extract was washed with saturated brine
4. 4
   건조the organic layer was dried over anhydrous magnesium sulfate
5. 5
   기타the solvent was evaporated under reduced pressure
6. 6
   기타The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

실험 절차

Under a nitrogen atmosphere, to a mixture of 1-(4-bromo-2-fluorophenyl)-3-methyl-1H-1,2,4-triazole (1.02 g), potassium carbonate (0.55 g) and potassium hexacyanoferrate(II) trihydrate (0.68 g) in DMF (4 mL)/ethanol (0.20 mL) was added palladium acetate (45 mg) at room temperature, and the mixture was stirred at 120° C. for 2 hr. The reaction mixture was allowed to cool to room temperature, and diluted with water and saturated brine, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, the organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (0.51 g).

출처