反应详情

With cooling with ice, ethyl 4-aminobutanoate hydrochloride (149 mg, 0.892 mmol) and diisopropylethylamine (303 μl, 1.78 mmol) were added to a dichloromethane (7 ml) solution of 2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (213 mg, 0.743 mmol), followed by stirring at room temperature for 15 hours. The reaction liquid was concentrated under reduced pressure, ethyl acetate was added, followed by washing with saturated brine. After drying over anhydrous sodium sulfate, the insoluble matter was separated by filtration, and the residue obtained by concentration was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=2:1→1:1, v/v) to obtain the entitled compound (279 mg, 99%) as a white solid.

1. customThe reaction liquid
2. concentrationwas concentrated under reduced pressure, ethyl acetate
3. additionwas added
4. washby washing 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. customwas purified by silica gel column chromatography (eluent, n-hexane