反应详情

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.21 g, 0.73 mmol), (diisopropylethylamine (0.28 ml, 1.65 mmol) and azetidine-3-carbonyldimethylamide hydrochloride (I-145) (0.25 g) were dissolved in dichloromethane (10 ml). After heated under reflux for 3 hours, this was diluted with dichloromethane, washed with water, then 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 dichloromethane:methanol=100:1) to obtain a colorless oil (0.24 g, 86%)

1. temperatureAfter heated
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 to dichloromethane:methanol=100:1)