反应详情

温度

100 °C

Compound 110g was synthesized using the same procedure as 103g, except using 110f (450 mg, 1.0 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (635 mg, 2.5 mmol), potassium acetate (393 mg, 4.0 mmol), bis(diphenylphosphino)-ferrocene]dichloropalladium(II) complex with CH2Cl2 (Pd Cl2dppf:CH2Cl2 (1:1), 66 mg, 0.08 mmol) and 1,4-dioxane (20 mL). The reaction mixture was heated at 100° C. for 5 h. The reaction mixture was cooled to room temperature and filtered through a pad of Celite 521. The filter cake was washed with Ethyl Acetate (2×25 mL), and the combined filtrates were concentrated to dryness under reduced pressure to afford 110g (quantitative yield) as black oil, which was used directly for the next step. MS (ESI+) m/z 497.3 (M+H).

1. customCompound 110g was synthesized
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationfiltered through a pad of Celite 521
4. washThe filter cake was washed with Ethyl Acetate (2×25 mL)
5. concentrationthe combined filtrates were concentrated to dryness under reduced pressure