反应详情

温度

80 °C

A solution of 4.12-A (100 mg, 0.2 mmol), 9-A (55 mg, 0.25 mmol), potassium carbonate (190 mg, 1.3 mmol) in 1,4-dioxane (1.5 mL) was added to a vial and degassed with nitrogen. Then [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1:1) (28 mg, 0.034 mmol) was added, degassed with nitrogen and the vial capped and heated at 80° C. overnight. The reaction mixture was filtered through silica gel and eluted with copious amounts of EtOAc. The solvent was concentrated and crude sample purified by reverse phase HPLC to afford 20 mg (15%) of 4.12-B. LCMS found for C24H30N2O4S2 (M+H)+: m/z=475.

1. customdegassed with nitrogen
2. customdegassed with nitrogen
3. customthe vial capped
4. filtrationThe reaction mixture was filtered through silica gel
5. washeluted with copious amounts of EtOAc
6. concentrationThe solvent was concentrated
7. customcrude sample purified by reverse phase HPLC