反应详情

温度

150 °C

4-[{4-Cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazol-2-yl}(methyl)amino]-N,N-dimethylbutanamide (I-156) (0.32 g, 0.81 mmol) was dissolved in dimethyl sulfoxide (5 ml), then triethylamine (0.24 ml, 1.73 mmol) and (3S)-3-(dimethylamino)pyrrolidine (0.21 ml, 1.66 mmol) were added, followed by stirring in a sealed tube at an external temperature of about 150° C. for 4 hours. This was diluted with dichloromethane, and washed with water and brine. After 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=20:1 to 10:1), then diisopropyl ether was added and the insoluble matter was collected by filtration to obtain a colorless solid (0.22 g, 56%).

1. washwashed with water and brine
2. dry with materialAfter drying over anhydrous sodium sulfate
3. customthe solvent was evaporated away under reduced pressure
4. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1 to 10:1)
5. additiondiisopropyl ether was added
6. filtrationthe insoluble matter was collected by filtration