반응 #158374

반응 방정식

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

ethyl acetate

water

ammonia

→

title compound

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

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   기타The organic layer was separated
2. 2
   세척washed with water and saturated brine
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   기타the solvent was evaporated under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

실험 절차

To a mixture of 1-(4-bromo-2-fluorophenyl)-3-methyl-1H-1,2,4-triazole (5.5 g), tris(dibenzylideneacetone)dipalladium(0) (393 mg), 1,1′-bis(diphenylphosphino)ferrocene (476 mg) and zinc powder (169 mg) in N,N-dimethylacetamide (20 mL) was added zinc(II) cyanide (1.5 g) at room temperature, and the mixture was stirred at 120° C. for 1 hr. To the reaction mixture were added ethyl acetate, water and aqueous ammonia. The organic layer was separated, washed with water and saturated brine, and 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 (3.84 g).

출처