تفاعل #158313

معادلة التفاعل

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

المذيبات

water

brine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool to room temperature
2. 2
   استخلاصthe mixture was extracted with ethyl acetate
3. 3
   غسيلThe extract was washed with saturated brine
4. 4
   تجفيفthe organic layer was dried over anhydrous magnesium sulfate
5. 5
   أخرىthe solvent was evaporated under reduced pressure
6. 6
   أخرىThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

الإجراء التجريبي

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).

المصدر