反应详情

温度

90 °C

To a solution of 4-hydroxy-2-nitroaniline (3.08 g, 20.0 mmol) in DMF (30 mL) was added NaH (60% oily, 880 mg, 22.0 mmol) followed by 1-fluoro-4-nitrobenzene (2.33 mL, 22.0 mmol). The mixture was stirred at 90° C. overnight. After cooling, the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, dried over Na2SO4 then evaporated. Sequence purification on SiO2 column chromatography gave the title compound (4.56 g, 83%): MS m/e 274 (M−1).

1. temperatureAfter cooling
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with water and brine
4. dry with materialdried over Na2SO4
5. customthen evaporated
6. customSequence purification on SiO2 column chromatography