反应详情

温度

110 °C

2-(Dimethylamino)-7-fluoro-5-methyl-6-(2-methyl-1,3-thiazol-4-yl)-1,3-benzoxazole-4-carbonitrile (I-171) (0.44 g, 1.39 mmol) was suspended in dimethyl sulfoxide (10 ml), then triethylamine (0.42 ml 3.03 mmol) and (3S)-3-(dimethylamino)pyrrolidine (0.38 ml, 3.00 mmol) were added, followed by stirring at an external temperature of about 110° C. for 4 hours. This was diluted with ethyl acetate, washed with water, and dried 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=50:1 to 10:1) to obtain a brown amorphous substance (0.51 g, 83%).

1. washwashed 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 (dichloromethane:methanol=50:1 to 10:1)
5. customto obtain a brown amorphous substance (0.51 g, 83%)