反应详情

温度

120 °C

A mixture of (±)-tert-butyl 3-methylpiperazine-1-carboxylate (1.5 g), 1-fluoro-4-nitrobenzene (1.06 g) and potassium carbonate (2.07 g) in dimethyl sulfoxide (15 ml) was stirred at 120° C. for 15 hours. The reaction mixture was cooled to room temperature and poured into water (30 ml). The mixture was extracted with ethyl acetate three times. The combined organic layers were washed successively with water (twice) and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate 2:1) to give the title compound as a white solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionThe mixture was extracted with ethyl acetate three times
3. washThe combined organic layers were washed successively with water (twice) and brine
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate 2:1)