反应详情

温度

50 °C

Diisopropylethylamine (169 μl, 0.944 mmol) and 2-(methylamino)pyridine (102 μl, 0.994 mmol) were added to a dichloromethane (10 ml) solution of 2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (190 mg, 0.663 mmol), followed by heating under reflux in an oil bath at 50° C. for 3 hours. The reaction liquid was cooled to room, temperature, ethyl acetate (70 ml) was added, followed by washing with water (50 ml) and saturated brine (50 ml). After drying over anhydrous sodium sulfate and concentration under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=4:1) to obtain the entitled compound (137 mg, 57.5%) as a colorless solid.

1. temperatureby heating
2. customThe reaction liquid
3. additionwas added
4. washby washing with water (50 ml) and saturated brine (50 ml)
5. dry with materialAfter drying over anhydrous sodium sulfate and concentration under reduced pressure
6. customthe resulting residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=4:1)