反应详情

温度

100 °C

To the compound (1.67 g, 4.72 mmol) obtained in Step 1, 7-bromo-4,5-difluoro-1-benzofuran (1.1 g, 4.72 mmol), sodium carbonate (1.0 g, 9.44 mmol), and Pd(dppf)Cl2 (catalytic amount), 1,4-dioxane (24 mL) and water (8 mL) were added, and stirred at 100° C. for 2 hours. The reaction solution was concentrated under reduced pressure. To the residue, ethyl acetate and 1 N hydrochloric acid were added and stirred. After that, the insoluble material was filtered off, and extraction was performed with ethyl acetate. The organic phase was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure, and the solid was collected by filtration.

1. concentrationThe reaction solution was concentrated under reduced pressure
2. additionTo the residue, ethyl acetate and 1 N hydrochloric acid were added
3. stirringstirred
4. filtrationAfter that, the insoluble material was filtered off
5. extractionextraction
6. washThe organic phase was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationThe solvent was distilled away under reduced pressure
9. filtrationthe solid was collected by filtration