反应详情

2,6-Dibromo-4-methylbenzaldehyde (600 g, 2.16 mmol), (2-fluorophenyl)hydrazine hydrochloride (351 mg, 2.16 mmol) and sodium acetate (180 mg, 2.19 mmol) were heated in methanol (15 mL) under reflux for 2 hours. The methanol was evaporated and the residue partitioned between dichloromethane (30 mL) and aqueous brine (30 mL). The organic phase was separated, combined with additional dichloromethane extracts (2×15 mL), washed with aqueous sodium bicarbonate (2×15 mL), passed through a hydrophobic frit and evaporated to the title compound (767 mg).

1. temperatureunder reflux for 2 hours
2. customThe methanol was evaporated
3. customthe residue partitioned between dichloromethane (30 mL) and aqueous brine (30 mL)
4. customThe organic phase was separated
5. washwashed with aqueous sodium bicarbonate (2×15 mL)
6. customevaporated to the title compound (767 mg)