反応 #158339

反応方程式

3,4-difluorophenol

potassium carbonate

ethyl 8-chloro-3-[3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)phenyl]-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridine-8-carboxylate

→

title compound

収率 44.1%

ethyl 8-(3,4-difluorophenoxy)-3-[3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)phenyl]-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridine-8-carboxylate

収率 44.1%

溶媒

DMF

ethyl acetate

ammonium chloride

反応条件

後処理

1. 1
   温度to cool to room temperature
2. 2
   洗浄the mixture was washed with saturated brine
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   その他the solvent was evaporated under reduced pressure
5. 5
   その他The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

実験手順

To a mixture of 3,4-difluorophenol (0.16 g) and potassium carbonate (0.50 g) in DMF (5 mL) was added ethyl 8-chloro-3-[3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)phenyl]-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridine-8-carboxylate (0.50 g) at room temperature, and the mixture was stirred at 100° C. for 30 min. The reaction mixture was allowed to cool to room temperature, and diluted with ethyl acetate and saturated aqueous ammonium chloride solution, the mixture was washed with 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 (0.27 g).

出典