反应详情

温度

60 °C

A mixture of 6-bromo-2-(4-tert-butoxycarbonylbenzyl)-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (2.54 g), palladium(II) acetate (52 mg), 1,1′-bis(diphenylphosphino)ferrocene (125 mg), triethylamine (1.6 ml), DMF (13 ml) and methanol (13 ml) was stirred at 60° C. for 72 hrs. under 1 atm carbon monoxide. The reaction mixture was concentrated and water was added to the residue. The mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-hexane:ethyl acetate=2:1) and recrystallized (ethyl acetate-hexane) to give the title compound (1.82 g).

1. concentrationThe reaction mixture was concentrated
2. additionwater was added to the residue
3. extractionThe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with water and saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography (hexane-hexane:ethyl acetate=2:1)
8. customrecrystallized (ethyl acetate-hexane)