反应详情

温度

110 °C

To a solution of compound 8A (3.0 g, 19.4 mmol) in DMF (40 mL) was added CsF (14.7 g, 96.8 mmol), followed by dibromoethane (1.84 mL, 21.3 mmol). The mixture was heated to 110° C. for 1.5 h, then cooled to rt, partitioned between water and Et2O. The separated Et2O layer was washed with water, saturated aqueous NaHCO3, brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with 5% MeOH in CH2Cl2 to afford the title compound (0.73 g).

1. temperaturecooled to rt
2. custompartitioned between water and Et2O
3. washThe separated Et2O layer was washed with water, saturated aqueous NaHCO3, brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was chromatographed (silica gel)
8. washeluting with 5% MeOH in CH2Cl2