反应详情

A mixture of 1-(4-(benzyloxy)-5-methoxy-2-nitrophenyl)ethanone (3.6 g, 12 mmol), iron powder (4.5 g) and ammonium formate (5.5 g) in toluene (50 mL) and water (50 mL) was heated at reflux temp. for 2 days with stirring. To this mixture was added EtOAc (100 mL), stirred for 20 minutes, the solid was filtered through a celite bed and washed with EtOAc (150 mL). The EtOAc layer was separated from the filtrate solution, washed with water (2×100 mL), dried over MgSO4 and concentrated in vacuo to afford the product (2.80 g, 86%) as a beige-colored solid. 1H NMR (CDCl3) δ 7.41-7.30 (m, 5H), 7.13 (s, 1H), 6.15 (br s, 2H), 6.10 (s, 1H), 5.13 (s, 2H), 3.84 (s, 3H), 2.51 (s, 3H).

1. temperaturewas heated
2. temperatureat reflux temp
3. stirringstirred for 20 minutes
4. filtrationthe solid was filtered through a celite bed
5. washwashed with EtOAc (150 mL)
6. customThe EtOAc layer was separated from the filtrate solution
7. washwashed with water (2×100 mL)
8. dry with materialdried over MgSO4
9. concentrationconcentrated in vacuo