反应详情

2-Isopropyl-4-nitro-benzoic acid 2-bromo-ethyl ester (0.19 g, 0.6 mmol) was dissolved in DMF (5 mL), then triethylamine (0.5 mL, 3.6 mmol) and 2-isopropylimidazole (0.2 g, 1.8 mmol) were added. The mixture was heated at reflux for 15 h then allowed to cool, diluted with water and extracted with ethyl acetate. The organic phase was washed with water and brine, dried over sodium sulfate and concentrated. The crude product was purified by column chromatography on silica gel (60-120 mesh), eluting with ethyl acetate, to afford 2-isopropyl-4-nitro-benzoic acid 2-(2-isopropyl-imidazol-1-yl)-ethyl ester (90 mg, 43%) as an oil.

1. temperatureThe mixture was heated
2. temperatureat reflux for 15 h
3. temperatureto cool
4. extractionextracted with ethyl acetate
5. washThe organic phase was washed with water and brine
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customThe crude product was purified by column chromatography on silica gel (60-120 mesh)
9. washeluting with ethyl acetate