反应详情

温度

150 °C

7-Fluoro-5-methyl-6-phenyl-2-(pyrrolidin-1-yl)-1,3-benzoxazole-4-carbonitrile (I-135) (0.10 g, 0.31 mmol) was suspended in dimethyl sulfoxide (3.5 ml), then triethylamine (90.0 μl, 0.65 mmol) and (3S)-3-(dimethylamino)pyrrolidine (88.0 μl, 0.69 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, washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified by preparative thin-layer chromatography (dichloromethane:methanol=20:1), then ether and a small amount of hexane were added, and the insoluble matter was collected by filtration to obtain a beige solid (38 mg, 29%).

1. washwashed with water and saturated brine
2. dry with materialdried over anhydrous sodium sulfate
3. customThe solvent was evaporated away under reduced pressure
4. customthe resulting residue was purified by preparative thin-layer chromatography (dichloromethane:methanol=20:1)
5. additionether and a small amount of hexane were added
6. filtrationthe insoluble matter was collected by filtration