反应详情

To a solution of 2-amino-3-nitrophenol (10 g) in dimethylformamide (100 ml) was added potassium carbonate (17.9 g) under ice-cooling, and the mixture was stirred for 30 minutes at the same temperature. To the mixture was added 4-methoxybenzyl chloride (10.7 g) at ambient temperature, and the mixture was stirred for 30 minutes under ice-cooling and then overnight at ambient temperature. To the reaction mixture was added water, and the mixture was extracted with dichloromethane, and purified by silica gel column chromatography (ethyl acetate-n-hexane). The residue was crystallized with ethanol to give 2-(4-methoxybenzyloxy)-6-nitroaniline (13.6 mg) as yellow needles.

1. temperaturecooling
2. stirringthe mixture was stirred for 30 minutes under ice-
3. temperaturecooling
4. customovernight
5. customat ambient temperature
6. extractionthe mixture was extracted with dichloromethane
7. custompurified by silica gel column chromatography (ethyl acetate-n-hexane)
8. customThe residue was crystallized with ethanol