反应详情

N-(2-Isopropyl-4-nitro-phenyl)-acetamide (3 g, 13.5 mmol) was dissolved in absolute ethanol (20 mL) and 5N hydrochloric acid (20 mL) was added. The mixture was heated to reflux overnight, cooled to r.t. then concentrated in vacuo to remove the ethanol. The mixture was basified with dilute sodium hydroxide solution and extracted with ethyl acetate. The combined organic layers were washed with water and brine solution, dried over sodium sulfate and concentrated. The crude product was purified by column chromatography on silica gel (60-120 mesh), eluting with 17% ethyl acetate/petroleum ether to afford 2-isopropyl-4-nitro-phenylamine (2.1 g, 85%).

1. temperatureThe mixture was heated
2. temperatureto reflux overnight
3. concentrationthen concentrated in vacuo
4. customto remove the ethanol
5. extractionextracted with ethyl acetate
6. washThe combined organic layers were washed with water and brine solution
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. customThe crude product was purified by column chromatography on silica gel (60-120 mesh)
10. washeluting with 17% ethyl acetate/petroleum ether