反应详情

温度

60 °C

2-Iodopropane (0.5 ml, 0.005 mol) was added to a suspension of methyl 3,4-dimethoxy-2-hydroxy-6-nitrobenzoate (1 g, 0.0039 mol) and sodium carbonate (1.6 g, 0.015 mol) in dimethylformamide (15 ml) and the reaction stirred at 60° C. for 2 hours. On cooling, the reaction was concentrated under reduced pressure and the residue partitioned between ethyl acetate (25 ml) and water (25 ml). The aqueous layer was further extracted with ethyl acetate (2×25 ml), the combined organic extracts dried (MgSO4), filtered and evaporated under reduced pressure to give the subtitle compound as a crystalline solid (1.1 g, 74%). 1H-NMR (CDCl3): δ=1.28 (6H, d), 3.94 (9H, m), 4.72 (1H, m), 7.49 (1H, s).

1. temperatureOn cooling
2. concentrationthe reaction was concentrated under reduced pressure
3. customthe residue partitioned between ethyl acetate (25 ml) and water (25 ml)
4. extractionThe aqueous layer was further extracted with ethyl acetate (2×25 ml)
5. dry with materialthe combined organic extracts dried (MgSO4)
6. filtrationfiltered
7. customevaporated under reduced pressure