反应详情

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-130) (0.20 g, 0.70 mmol) was dissolved in dichloromethane (10 ml), then ethyl isonipecotate (0.12 ml, 0.78 mmol) and diisopropylethylamine (0.15 ml, 0.88 mmol) were added, followed by heating under reflux for 3 hours. This was diluted with dichloromethane, washed with water, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=100:1) to obtain a yellow oil (0.27 g, 94%).

1. temperatureby heating
2. temperatureunder reflux for 3 hours
3. washwashed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated away under reduced pressure
6. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=100:1)