反应详情

温度

95 °C

2-Cyclopentyl-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-275) (112 mg, 0.24 mmol) was dissolved in dimethyl sulfoxide (5 ml), then triethylamine (100 μl, 0.36 mmol) and (3S)-3-(dimethylamino)pyrrolidine (93 μl, 0.31 mmol) were added, followed by stirring under nitrogen atmosphere at 95° C. for 4 hours. After cooling, this was concentrated under reduced pressure, diluted, with chloroform, washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate, then the solvent was evaporated away under reduced pressure. The resulting residue was purified by preparative TLC (chloroform:methanol=10:1, v/v) to obtain the entitled compound (48 mg, 33%) as a white crystal.

1. temperatureAfter cooling
2. concentrationthis was concentrated under reduced pressure
3. additiondiluted, with chloroform
4. washwashed with saturated brine
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. customthe solvent was evaporated away under reduced pressure
7. customThe resulting residue was purified by preparative TLC (chloroform