反应详情

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.49 g, 1.71 mmol), diisopropylethylamine (0.70 ml, 4.12 mmol) and ethyl 3-(methylamino)propionate hydrochloride (I-159) (0.32 g, 1.91 mmol) were dissolved in dichloromethane (15 ml). After heated under reflux for 3 hours, this was diluted with dichloromethane. After washed 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 to dichloromethane:methanol=70; 1), then again purified by silica gel column chromatography (hexane:ethyl acetate=4:1 to 2:1) to obtain the entitled compound (0.53 g, 81%) as a brown oil.

1. temperatureAfter heated
2. temperatureunder reflux for 3 hours
3. washAfter washed 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)
7. customagain purified by silica gel column chromatography (hexane:ethyl acetate=4:1 to 2:1)