反应详情

温度

90 °C

To a solution of 2-hydroxy-3-methoxy-4-nitro-benzaldehyde (10.4 g, 52.8 mmol, prepared as described in: J. Heterocyclic Chem., 1996, 33, 1171-78) in DMF (100 ml) was added potassium carbonate (11.04 g, 80 mmol), followed by methyl iodide (4 mL, 64 mmol) and the mixture stirred at 90° C. for 1 hour. The mixture was partitioned between ethyl acetate and water, separated, the organic phase was washed with brine, dried (Na2SO4), filtered, and the solvents were removed in vacuo. The resulting residue was subjected to flash chromatography (SiO2, 20% ethyl acetate in cyclohexane) to give the title compound as a yellow oil (8.2 g, 74%). LCMS (Method B): RT=3.76 min, [M+H]+=212.

1. customThe mixture was partitioned between ethyl acetate and water
2. customseparated
3. washthe organic phase was washed with brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customthe solvents were removed in vacuo