反应详情

温度

110 °C

(3S)-3-(Dimethylamino)pyrrolidine (53 μl, 0.42 mmol) and triethylamine (100 μl) were added to a dimethyl sulfoxide (2 ml) solution of 7-fluoro-5-methyl-2-(1-methyl-1H-pyrrol-2-yl)-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-166) (69 mg, 0.21 mmol). The system was purged with nitrogen, then sealed up, and heated at 110° C. for 3.5 hours. After cooling, the solvent was evaporated away under reduced pressure, the resulting residue was dissolved in chloroform and washed with water. The organic layer was dried over anhydrous sodium sulfate, then the solvent was evaporated away under reduced pressure, and the resulting residue was separated and purified by preparative TLC to obtain a main product. This was washed with a mixed solvent of isopropyl ether and ethanol, and the solid was collected by filtration to obtain the entitled compound (24 mg, 27%) 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
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. customthe solvent was evaporated away under reduced pressure
9. customthe resulting residue was separated
10. custompurified by preparative TLC
11. customto obtain a main product
12. washThis was washed with a mixed solvent of isopropyl ether and ethanol
13. filtrationthe solid was collected by filtration