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 (0.15 ml, 0.88 mmol) and N-methyl-tert-butylamine (0.10 ml, 0.84 mmol) were added. After heating under reflux for 3 hours, N-methyl-tert-butylamine (50.0 μl, 0.42 mmol) was added, followed by heating under reflux for 2 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) to obtain a pale yellow solid (0.22 g, 0.65 mmol, 93%).

1. temperatureAfter heating
2. temperatureunder reflux for 3 hours
3. temperatureby heating
4. temperatureunder reflux for 2 hours
5. washwashed with water
6. dry with materialdried 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)