反应详情

A mixture of 5-bromo-6-chloro-1H-indole-3-carbaldehyde (200 mg, 0.77 mmol), phenyl boronic acid (114 mg, 0.93 mmol), 2N aqueous potassium carbonate (1.15 mL, 3.10 mmol) in toluene (3.3 mL) and EtOH (1.1 mL) was degassed with N2, treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (56.6 mg, 0.077 mmol), and degassed again with N2. The mixture was subjected to microwave irradiation conditions at 120° C. for 30 minutes. The reaction mixture was cooled to room temperature, diluted with water and extracted with EtOAc (50 mL). The organic layer was washed with brine, dried over MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography (0-46% EtOAc/petroleum ether) to afford the title compound (190 mg, 98% yield) as a yellow solid.

1. customwas degassed with N2
2. customdegassed again with N2
3. customirradiation conditions at 120° C. for 30 minutes
4. additiondiluted with water
5. extractionextracted with EtOAc (50 mL)
6. washThe organic layer was washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. customThe crude material was purified by flash chromatography (0-46% EtOAc/petroleum ether)