反应详情

6-Bromo-2-chloro-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile (I-167) (1.93 g, 6.67 mmol) was dissolved in dichloromethane (40 ml), then diisopropylethylamine (1.20 ml, 7.06 mmol) and dimethylamine (2.0 M tetrahydrofuran solution, 5.00 ml, 10.0 mmol) were added. After stirring with heating under reflux overnight, this was diluted with dichloromethane. After washing with water and drying over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure, then the resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1) to obtain a yellow solid (1.12 g, 56%).

1. temperaturewith heating
2. temperatureunder reflux overnight
3. washAfter washing with water
4. dry with materialdrying 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 to dichloromethane:methanol=70:1)