反应详情

温度

50 °C

To a solution of ethyl 4-bromo-2-methyl-2-(methylsulfonyl)butanoate (2.08 g, 7.25 mmol) and 4-iodo-3-methylpyridin-2(1H)-one (1.42 g, 6.04 mmol) in tetrahydrofuran (60.4 mL) was added cesium carbonate (4.06 g, 12.1) at ambient temperature. The resulting mixture was stirred at 50° C. overnight. The mixture was allowed to cool to ambient temperature and filtered through a celite pad. The pad was washed with ethyl acetate and the filtrate was concentrated to a crude residue. The material was purified via filtration through a silica gel pad, eluting with heptanes/ethyl acetate. The desired fractions were isolated, the solvent removed via rotary evaporation affording ethyl 4-(4-iodo-3-methyl-2-oxopyridin-1(2H)-yl)-2-methyl-2-(methylsulfonyl)butanoate as an oil. 1.97 g

1. temperatureto cool to ambient temperature
2. filtrationfiltered through a celite pad
3. washThe pad was washed with ethyl acetate
4. concentrationthe filtrate was concentrated to a crude residue
5. filtrationThe material was purified via filtration through a silica gel pad
6. washeluting with heptanes/ethyl acetate
7. customThe desired fractions were isolated
8. customthe solvent removed via rotary evaporation