反应详情

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (0.45 g, 1.57 mmol) was dissolved in dichloromethane (15 ml), then diisopropylethylamine (0.6 ml, 3.53 mmol) and ethyl azetidine-3-carboxylate hydrochloride (I-147) (0.55 g) were 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 to dichloromethane:methanol=70:1) to obtain a brown oil (0.60 g, quant).

1. temperatureAfter heated
2. temperatureunder reflux for 3 hours
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)
7. customto obtain a brown oil (0.60 g, quant)