反应详情

Dibromoisocyanuric acid (24.8 g) was added to a solution of 2,4′-difluoro-3-hydroxybiphenyl-4-carbaldehyde (33.7 g) in DMF (400 mL) at room temperature. The mixture was stirred at the same temperature under nitrogen atmosphere for 3 hours. The mixture was quenched with aqueous saturated sodium thiosulfate solution at room temperature and extracted with ethyl acetate. The organic layer was separated, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by a silica gel column chromatography (hexane/ethyl acetate) to give the title compound (33.1 g).

1. customThe mixture was quenched with aqueous saturated sodium thiosulfate solution at room temperature
2. extractionextracted with ethyl acetate
3. customThe organic layer was separated
4. washwashed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by a silica gel column chromatography (hexane/ethyl acetate)