反应详情

温度

90 °C

To a single necked round bottomed flask fitted with stop cock with N2(g) balloon, in DMF was added Methyl 3-(benzyloxy)-5-hydroxybenzoate (24 g) (Intermediate 12). Under stirring, potassium carbonate (38 g) followed by 4-fluorobenzaldehyde (13.84 g) were added at room temperature. The reaction was heated at 90° C. for 16 h with constant stirring. The reaction mixture was diluted with water and extracted with EtOAc. All organic layers were combined and washed with water, brine, dried over anhydrous sodium sulphate, filtered and concentrated under vacuum to get crude thick liquid product. The crude product was purified by flash column chromatography to yield title compound (32.5 g).

1. additionwere added at room temperature
2. extractionextracted with EtOAc
3. washwashed with water, brine
4. dry with materialdried over anhydrous sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customto get crude thick liquid product
8. customThe crude product was purified by flash column chromatography