反应详情

温度

150 °C

(3S)-3-(dimethylamino)pyrrolidine (161 μl, 1.27 mmol) and triethylamine (177 μl, 1.27 mmol) were added to a dimethyl sulfoxide (9 ml) solution of tert-butyl N-(4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazol-2-yl)-β-alaninate (I-278) (335 mg, 0.847 mmol), followed by stirring in an oil bath at 150° C. for 5 hours. The reaction liquid was concentrated under reduced pressure, the residue was dissolved in ethyl acetate and washed with water and saturated brine. After drying over anhydrous sodium sulfate, the insoluble matter was separated by filtration, the residue obtained by concentration was purified by silica gel column chromatography (eluent, chloroform:methanol=20:1, v/v) to obtain the entitled compound (120 mg, 29%) as a brown oily substance.

1. customThe reaction liquid
2. concentrationwas concentrated under reduced pressure
3. dissolutionthe residue was dissolved in ethyl acetate
4. washwashed with water and 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. customwas purified by silica gel column chromatography (eluent, chloroform