反应详情

温度

95 °C

A mixture of 3-fluoro-4-(methylsulfonyl)nitrobenzene (8 g, 36.5 mmol), iron powder (22 g, 394 mmol), and acetic acid (0.3 mL) in water (200 mL) was heated at 95° C. for 3 hours. After cooling, insolubles were filtered off by Celite. The filtrate was extracted with ethyl acetate (200 mL×2), the combined organic layer washed with water, brine, dried over MgSO4, and concentrated in vacuo. Chromatographic purification of the residue eluting with ethyl acetate/hexane (1/1) provided the subtitle compound (6.2 g, 90% yield).

1. temperatureAfter cooling
2. filtrationinsolubles were filtered off by Celite
3. extractionThe filtrate was extracted with ethyl acetate (200 mL×2)
4. washthe combined organic layer washed with water, brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customChromatographic purification of the residue
8. washeluting with ethyl acetate/hexane (1/1)