反应详情

温度

60 °C

To a solution of 5-nitrosalicylaldehyde (1.00 g, 6.0 mmol) in DMF (20 ml) was added NaH (246 mg) and methyl iodide (2.56 g, 18 mmol) at 0° C. The mixture was stirred for 8.5 hr at 60° C. After the reaction mixture was extracted with ether, the extract was washed with aqueous NaHCO3, brine and 5%-HCl/aq.NaCl, dried over MgSO4 and concentrated in vacuo to afford 2-methoxy-5-nitrobenzaldehyde (0.95 g, 87.8%) as a yellow needle.

1. extractionAfter the reaction mixture was extracted with ether
2. washthe extract was washed with aqueous NaHCO3, brine and 5%-HCl/aq
3. dry with materialNaCl, dried over MgSO4
4. concentrationconcentrated in vacuo