反应详情

温度

90 °C

2-(1-Acetylpiperidin-4-yl)-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-104) (0.23 g, 0.61 mmol) was dissolved in dimethyl sulfoxide (7 ml), triethylamine (0.18 ml, 1.30 mmol) and (3S)-3-(dimethylamino)pyrrolidine (85.0 μl, 0.67 mmol) were added, followed by stirring an external temperature of about 90° C. for 4 hours. After dilution with ethyl acetate, this was washed with water, dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure and the resulting residue was purified by silica gel column chromatography (silica gel 10 g, dichloromethane:methanol=30:1) to obtain a colorless oil (73 mg, 25%). This was dissolved in dioxane and freeze-dried into solid.

1. washAfter dilution with ethyl acetate, this was washed with water
2. dry with materialdried over anhydrous sodium sulfate
3. customThe solvent was evaporated away under reduced pressure
4. customthe resulting residue was purified by silica gel column chromatography (silica gel 10 g, dichloromethane:methanol=30:1)