反应详情

温度

90 °C

(3S)-3-(Dimethylamino)pyrrolidine (157 μl, 1.24 mmol) and triethylamine (348 μl, 2.50 mmol), were added to a dimethyl sulfoxide (5 ml) solution of 6-bromo-2-cyclopropyl-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile (I-77) (304 mg, 1.03 mmol). The system was purged with nitrogen and then sealed up and heated at 90° C. for 2 hours. After cooling, the solvent was evaporated away under reduced pressure, then the resulting residue was dissolved in chloroform, washed with water and saturated brine. The organic layer was dried over anhydrous sodium sulfate, then the solvent was evaporated away under reduced pressure, the resulting residue was washed with a mixed solvent of isopropyl ether and ethanol. The crystal was collected by filtration to obtain the entitled compound (106 mg, 26%) as a colorless solid.

1. customThe system was purged with nitrogen
2. customsealed up
3. temperatureAfter cooling
4. customthe solvent was evaporated away under reduced pressure
5. dissolutionthe resulting residue was dissolved in chloroform
6. washwashed with water and saturated brine
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. customthe solvent was evaporated away under reduced pressure
9. washthe resulting residue was washed with a mixed solvent of isopropyl ether and ethanol
10. filtrationThe crystal was collected by filtration