反应详情

2,6-Dibromo-4-methylbenzaldehyde (89.5 g, 0.322 mol), (2,4-difluorophenyl)hydrazine hydrochloride (58.25 g, 0.322 mol) and sodium acetate (26.9 g, 0.328 mol) were heated in methanol (1.25 L) at reflux for 3.5 hours. The mixture was cooled and the precipitate was collected by filtration and partitioned between ethyl acetate (750 mL) and water (250 mL). The ethyl acetate layer was combined with a second ethyl acetate extract, washed successively with water and brine, dried over anhydrous sodium sulphate and evaporated under reduced pressure to afford the title compound as an off-white solid (97.5 g).

1. temperatureat reflux for 3.5 hours
2. temperatureThe mixture was cooled
3. filtrationthe precipitate was collected by filtration
4. custompartitioned between ethyl acetate (750 mL) and water (250 mL)
5. extractionextract
6. washwashed successively with water and brine
7. dry with materialdried over anhydrous sodium sulphate
8. customevaporated under reduced pressure