反应详情

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.20 g, 0.70 mmol) was dissolved in dichloromethane (10 ml), and diisopropylethylamine (0.13 ml, 0.76 mmol) and N-methylethanolamine (62.0 μl, 0.78 mmol) were added. After heating under reflux for 3 hours, N-methylethanolamine (62.0 μl, 0.78 mmol) was added. After heated under reflux for 3 hours, this was diluted with dichloromethane. After washing with water and drying 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=40:1) to obtain a pale yellow oil (0.21 g, 93%).

1. temperatureAfter heating
2. temperatureunder reflux for 3 hours
3. temperatureAfter heated
4. temperatureunder reflux for 3 hours
5. washAfter washing with water
6. dry with materialdrying over anhydrous sodium sulfate
7. customthe solvent was evaporated away under reduced pressure
8. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=40:1)