反应详情

温度

50 °C

Treat a mixture of 1-(2-bromo-4-fluoro-5-nitrophenyl)propan-2-one (12 g, 43.6 mmol) in acetic acid (200 mL) with iron powder (24 g, 0.436 mol) and stir at 50° C. for 1 h. Add water and EtOAc, filter to remove solids, and extract the filtrate with EtOAc (2×). Wash the combined organics with saturated. Na2CO3, then brine, dry over Na2SO4 and concentrate to dryness to afford the title compound (10.2 g, 94% yield). 1H NMR (400 MHz, DMSO-d6): δ 7.26 (d, J=10.8 Hz, 1H), 6.69 (d, J=9.6 Hz, 1H), 5.33 (s, 2H), 3.74 (s, 2H), 2.14 (s, 3H).

1. additionTreat
2. filtrationAdd water and EtOAc, filter
3. customto remove solids
4. extractionextract the filtrate with EtOAc (2×)
5. washWash the combined organics with saturated
6. dry with materialNa2CO3, then brine, dry over Na2SO4
7. concentrationconcentrate to dryness