反应详情

[1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium (II) (416 mg), triethylamine (1.59 mL) and methanol (6.91 mL) was added to a solution of tert-butyl 4-(4-iodo-3-methyl-2-oxopyridin-1(2H)-yl)piperidine-1-carboxylate (2.38 g) in DMF (15 mL) at room temperature. The mixture was stirred at 90 C under 0.5 MPa of carbon monoxide atmosphere for 7 hours. The mixture was quenched with water at room temperature and filtrated through celite. The filtrate was extracted with ethyl acetate. The organic layer was separated, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was passed through a silica gel (NH, hexane/ethyl acetate) and concentrated in vacuo. The residue was triturated with diisopropyl ether/hexane and collected by filtration to give the title compound (1.77 g).

1. customThe mixture was quenched with water at room temperature
2. filtrationfiltrated through celite
3. extractionThe filtrate was extracted with ethyl acetate
4. customThe organic layer was separated
5. washwashed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. concentrationconcentrated in vacuo
9. customThe residue was triturated with diisopropyl ether/hexane
10. filtrationcollected by filtration