反应详情

Tert-butyl 4-(((4-methylphenyl)sulfonyl)oxy)piperidine-1-carboxylate (21.7 g) was added to a mixture of 4-iodo-3-methylpyridin-2(1H)-one (8.98 g) and potassium carbonate (21.1 g) in 1-methoxy-2-(2-methoxyethoxyl)ethane (160 mL) at room temperature. The mixture was stirred at 100 C under nitrogen atmosphere for 22 hours. The mixture was quenched with water at room temperature and extracted with ethyl acetate. The organic layer was separated, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. Toluene was added to the residue. The mixture was concentrated in vacuo. The residue was purified by a silica gel column chromatography (hexane/ethyl acetate) to give the title compound (12.9 g).

1. customThe mixture was quenched with water at room temperature
2. extractionextracted with ethyl acetate
3. customThe organic layer was separated
4. washwashed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo
7. additionToluene was added to the residue
8. concentrationThe mixture was concentrated in vacuo
9. customThe residue was purified by a silica gel column chromatography (hexane/ethyl acetate)