反应详情

温度

65 °C

A mixture of iron powder (8.8 g, 158 mmol), water (60 mL) and hydrochloric acid (2 mL) was stirred at 65° C. for 20 min. It was then cooled to rt and the aqenous layer was poured out. A solution of 4-(2-fluoro-4-nitrophenyl)morpholin-3-one (3.8 g, 15.8 mmol) in MeOH (100 mL) was added and the resuting mixture was acidified to pH 2 with hydrochloric acid and stirred at 65° C. for 4 h. The mixture was cooled to rt, adjusted to pH 8 with saturated NaHCO3 aqueous solution and filtered. The MeOH was removed in vacuo and the mixture was extracted with EtOAc (20 mL×3). The combined organic layers were washed with brine (20 mL×4), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:2) to give the title compound as a white solid (1.89 g, 57%).

1. temperatureIt was then cooled to rt
2. additionthe aqenous layer was poured out
3. stirringstirred at 65° C. for 4 h
4. temperatureThe mixture was cooled to rt
5. filtrationfiltered
6. customThe MeOH was removed in vacuo
7. extractionthe mixture was extracted with EtOAc (20 mL×3)
8. washThe combined organic layers were washed with brine (20 mL×4)
9. dry with materialdried over anhydrous Na2SO4
10. concentrationconcentrated in vacuo
11. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:2)