反应详情

Cesium carbonate (17.65 g, 54.2 mmol) and 4-(bromomethyl)-1,2-difluorobenzene (5.78 ml, 45.1 mmol) were added to a solution of 5-formyl-2-hydroxybenzoic acid (3 g, 18.06 mmol) in dimethylformamide (100 ml) was added) at room temperature. The mixture was stirred at room temperature overnight. The mixture was then filtered, the dimethylformamide was evaporated and the residue was diluted with ethyl acetate (100 ml) and washed with water (3×50 ml). The organic layer was dried (MgSO4) and evaporated under reduced pressure to give an oil which solidified on standing solidified. The solid was triturated with an 8:1 mixture of hexane/ethyl acetate. The solid was filtered and dried in air under vacuum to yield the title compound as a white solid. 7 g.

1. additionwas added) at room temperature
2. filtrationThe mixture was then filtered
3. customthe dimethylformamide was evaporated
4. additionthe residue was diluted with ethyl acetate (100 ml)
5. washwashed with water (3×50 ml)
6. dry with materialThe organic layer was dried (MgSO4)
7. customevaporated under reduced pressure
8. customto give an oil which
9. customThe solid was triturated with an 8:1 mixture of hexane/ethyl acetate
10. filtrationThe solid was filtered
11. customdried in air under vacuum