反应详情

A mixture of tris(dibenzylideneacetone)dipalladium(0) (157 mg), 1,1′-bis(diphenylphosphino)ferrocene (380 mg) and N,N-dimethylformamide (10 mL) was stirred under an argon atmosphere for 10 minutes. To the mixture were added (5-benzyloxy-2-iodo-4-methoxyphenyl)piperidin-1-yl-methanone (reference example 6-1) (1.55 g), 2-propanol (10 mL) and triethylamine (1.44 mL). After displacement to a carbon monoxide atmosphere, the mixture was stirred at 90° C. for 14 hours. After cooling to room temperature, to the mixture were added ethyl acetate and 2 mol/L hydrochloric acid. The separated organic layer was washed with water, a 2 mol/L aqueous solution of sodium hydroxide, an aqueous solution of sodium bicarbonate and brine successively, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: 15%-45% ethyl acetate/hexane, gradient elution) to give the title compound (258 mg).

1. washThe separated organic layer was washed with water
2. dry with materiala 2 mol/L aqueous solution of sodium hydroxide, an aqueous solution of sodium bicarbonate and brine successively, dried over anhydrous magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by silica gel column chromatography (eluent: 15%-45% ethyl acetate/hexane, gradient elution)