反应详情

温度

120 °C

A solution of 5-fluor-2-nitrobenzoic acid (2.6 g, 14.1 mmol, Aldrich Chemical Co., Milwaukee, Wis.) and phenol (1.5 g, 15.5 mmol, Aldrich Chemical Co., Milwaukee, Wis.) in DMF (70 mL) was treated with K2CO3 (5.9 g, 42.4 mmol) and heated to 120° C. for 6 hours. The reaction was cooled to room temperature and the solvent removed under reduced pressure. The resulting residue was dissolved in water and extracted with EtOAc. The combined organic layers were washed with saturated aqueous NaCl, dried (Na2SO4), filtered, and concentrated to afford 34A (4.5 g).

1. temperatureThe reaction was cooled to room temperature
2. customthe solvent removed under reduced pressure
3. dissolutionThe resulting residue was dissolved in water
4. extractionextracted with EtOAc
5. washThe combined organic layers were washed with saturated aqueous NaCl
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated