反应详情

温度

150 °C

(3S)-3-(Dimethylamino)pyrrolidine (55 μl, 0.435 mmol) and triethylamine (70 μl, 0.502 mmol) were added to a dimethyl sulfoxide (3 ml) solution of 7-fluoro-5-methyl-2-morpholin-4-yl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-283) (113 mg, 0.335 mmol), followed by stirring in an oil bath at 150° C. for 2 hours. The reaction liquid was concentrated under reduced pressure, the residue was dissolved in chloroform and washed with saturated brine. After drying over anhydrous sodium sulfate, the insoluble matter was separated by filtration, the residue obtained by concentration was preparative TLC (eluent, chloroform:methanol=10:1, v/v), and the obtained eluate was recrystallized from hot ethanol to obtain the entitled compound (33.0 mg, 22%) as a white solid.

1. customThe reaction liquid
2. concentrationwas concentrated under reduced pressure
3. dissolutionthe residue was dissolved in chloroform
4. washwashed with saturated brine
5. dry with materialAfter drying over anhydrous sodium sulfate
6. customthe insoluble matter was separated by filtration
7. customthe residue obtained by concentration
8. custommethanol=10:1, v/v), and the obtained eluate was recrystallized from hot ethanol