反应详情

温度

100 °C

A screw-cap vial was charged with 66.15D (2.08 g, 5.39 mmol), 1,4-dioxane (20 mL), and dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium(II) DCM adduct (available from Strem) (0.220 g, 0.269 mmol). The suspension was sparged with N2, and to it were added TEA (2.25 mL, 16.2 mmol) and 4,4,5,5-tetramethyl-1,3,2-dioxaborolane (available from Aldrich) (1.17 mL, 8.08 mmol). The resulting mixture was stirred overnight at 100° C. (sealed vial), cooled to room temperature, diluted with water, and extracted with EtOAc. The combined organic layers were washed with water, 1 N HCl, and brine, dried (MgSO4), and concentrated. The crude product was twice purified by silica gel flash chromatography (0-15% EtOAc/hexane) to afford 66.56A (1.09 g, 52% yield) as a crystalline white solid.

1. customThe suspension was sparged with N2
2. custom(sealed vial)
3. temperaturecooled to room temperature
4. extractionextracted with EtOAc
5. washThe combined organic layers were washed with water, 1 N HCl, and brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customThe crude product was twice purified by silica gel flash chromatography (0-15% EtOAc/hexane)