反应详情

2,4-Dibromo-5-hydroxy-benzaldehyde (50 g, 178.6 mmol), 1,2-difluoro-4-nitrobenzene (28.4 g, 178.6 mmol) and potassium carbonate (49.0 g, 357.2 mmol) are stirred in DMF (500 mL) at 60° C. for 2 hours. The reaction is quenched with water (1000 mL) and extracted with methyl tert-butylether (MTBE) (2×500 mL). The organic layer is washed with saturated sodium chloride aqueous solution (2×500 mL), dried with anhydrous sodium sulfate, and concentrated to obtain a yellow solid. The crude solid is recrystallized in EtOAc/PE (1:5) to give 2,4-dibromo-5-(2-fluoro-4-nitrophenoxy)benzaldehyde as a yellow solid (52.8 g, 70.6% yield).

1. customThe reaction is quenched with water (1000 mL)
2. extractionextracted with methyl tert-butylether (MTBE) (2×500 mL)
3. washThe organic layer is washed with saturated sodium chloride aqueous solution (2×500 mL)
4. dry with materialdried with anhydrous sodium sulfate
5. concentrationconcentrated
6. customto obtain a yellow solid
7. customThe crude solid is recrystallized in EtOAc/PE (1:5)