反应详情

温度

85 °C

Reduced iron (150 mg, 2.69 mmol) was added to a solution of [(6-{(4S)-4-[(tert-butoxycarbonyl)amino]-2-oxopyrrolidin-1-yl}-2-nitropyridin-3-yl)oxy]acetic acid ethyl ester (380 mg, 0.895 mmol) in acetic acid (3.8 ml) and the mixture was stirred at 85° C. for 1.5 hours. After cooling, the insoluble material was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was dissolved in dichloromethane, a saturated sodium hydrogen carbonate aqueous solution was added thereto and the mixture was stirred for 10 minutes. The solvent was removed under reduced pressure and the obtained residue was purified by silica gel column chromatography (chloroform/methanol) to yield 305 mg (98%) of the title compound in the form of a colorless solid.

1. temperatureAfter cooling
2. customthe insoluble material was removed by filtration
3. concentrationthe filtrate was concentrated under reduced pressure
4. dissolutionThe residue was dissolved in dichloromethane
5. additiona saturated sodium hydrogen carbonate aqueous solution was added
6. stirringthe mixture was stirred for 10 minutes
7. customThe solvent was removed under reduced pressure
8. customthe obtained residue was purified by silica gel column chromatography (chloroform/methanol)