反应详情

温度

90 °C

The compound (279 mg, 0.447 mmol) obtained in Example 14a was dissolved in N,N-dimethylformamide (3 mL), and palladium acetate (15 mg, 0.0671 mmol), 1,1′-bis(diphenylphosphino)ferrocene (74 mg, 0.134 mmol), triethylamine (1.24 mL, 8.94 mmol) and benzyl alcohol (0.926 mL, 8.94 mmol) were added. The atmosphere in the system was replaced with a carbon monoxide atmosphere, the mixture was stirred at 90° C. for 17.5 hours, then palladium acetate (30 mg, 0.134 mmol) and 1,1′-bis(diphenylphosphino)ferrocene (148 mg, 0.268 mmol) were added, and the mixture was stirred at 90° C. under the carbon monoxide atmosphere for 29 hours. Palladium acetate (30 mg, 0.134 mmol) and 1,1′-bis(diphenylphosphino)ferrocene (148 mg, 0.268 mmol) were added, and the mixture was stirred at 90° C. under the carbon monoxide atmosphere for 60 hours. The reaction mixture was diluted with ethyl acetate, insoluble matter was removed by filtration through celite, then the solvent was evaporated under reduced pressure, and the resulting residue was purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1→1:2, v/v) to give the title compound (182 mg; yield, 60%) as a brown oily substance.

1. customwas removed by filtration through celite
2. customthe solvent was evaporated under reduced pressure
3. customthe resulting residue was purified by NH silica gel column chromatography (hexane