反应详情

温度

130 °C

(3S)-3-(Dimethylamino)pyrrolidine (67.9 μl, 0.535 mmol) and triethylamine (86.1 μl, 0.618 mmol) were added to a dimethyl sulfoxide (5 ml) solution of 7-fluoro-5-methyl-2-(4-methyl-3-oxopiperazin-1-yl)-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-188) (150 mg, 0.412 mmol), followed by stirring in an oil bath at 130° C. for 3 hours. The reaction liquid was concentrated under reduced pressure, the residue was dissolved in chloroform (50 ml), washed with saturated brine (50 ml). After drying over anhydrous sodium sulfate and concentration, the resulting residue was purified by preparative TLC (eluent, chloroform:methanol=10:1) to obtain the entitled compound (109 mg, 54.5%) as a colorless foamy substance.

1. customThe reaction liquid
2. concentrationwas concentrated under reduced pressure
3. dissolutionthe residue was dissolved in chloroform (50 ml)
4. washwashed with saturated brine (50 ml)
5. dry with materialAfter drying over anhydrous sodium sulfate and concentration
6. customthe resulting residue was purified by preparative TLC (eluent, chloroform:methanol=10:1)