反应详情

To a suspension of phenylamine L (465 mg, 5.0 mmol) and potassium phosphate (530 mg, 2.5 mmol) in acetonitrile (20 mL) was added 2,4-dibromo-butyryl chloride III (1.32 g, 5.0 mmol) at 0° C. The mixture was brought to rt and stirred for 1 hr. Then NaOH (1 mL, 50% aqueous solution) was added, and the mixture was stirred overnight. After the mixture was filtered, the solid was washed with acetonitrile (10 mL), and the combined filtrate was concentrated. The residue was purified by column chromatography (eluate: EtOAc/petroleum ether from 1/5 to 1/3) to afford 3-bromo-1-phenyl-pyrrolidin-2-one LI as white solid.

1. customwas brought to rt
2. stirringthe mixture was stirred overnight
3. filtrationAfter the mixture was filtered
4. washthe solid was washed with acetonitrile (10 mL)
5. concentrationthe combined filtrate was concentrated
6. customThe residue was purified by column chromatography (eluate: EtOAc/petroleum ether from 1/5 to 1/3)