反应详情

温度

60 °C

2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-130) (0.11 g, 0.38 mmol) was dissolved in a mixed solvent of dichloromethane (10 ml) and ethanol (7 ml), then diisopropylethylamine (0.21 ml, 1.23 mol) and azetidine hydrochloride (71.5 mg, 0.76 mmol) were added. After stirring at an external temperature of about 60° C. for 3 hours, the reaction liquid was concentrated under reduced pressure and 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:methanol=100:1) to obtain a colorless solid (85 mg, 74%).

1. customthe reaction liquid
2. concentrationwas concentrated under reduced pressure
3. additiondiluted with dichloromethane
4. washAfter washing with water
5. dry with materialdrying over anhydrous sodium sulfate
6. customthe solvent was evaporated away under reduced pressure
7. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=100:1)