反应详情

To a solution of 109c (3.5 g, 15 mmol) in N,N-dimethylformamide (30 mL) was added potassium carbonate (4.14 g, 30 mmol) and iodomethane (1.4 mL, 22.7 mmol). The reaction was stirred at room temperature for overnight. Water (50 mL) was added to quench the reaction and the resulting mixture was extracted with ethyl acetate (5 mL×3). The combined organic phase was dried over anhydrous Na2SO4, filtered, and evaporated under reduced pressure. The residue was purified by column chromatography eluting with petroleum ether/ethyl acetate (from 4:1 to 1:2) to afford 109d as a white solid (1.4 g, 38%). LCMS: [M+H]+ 245/247. 1H NMR (500 MHz, CDCl3) δ 7.89 (s, 1H), 7.46 (d, J=2.0 Hz, 1H), 7.32 (d, J=2.0 Hz, 1H), 3.81 (s, 3H).

1. customto quench
2. customthe reaction
3. extractionthe resulting mixture was extracted with ethyl acetate (5 mL×3)
4. dry with materialThe combined organic phase was dried over anhydrous Na2SO4
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customThe residue was purified by column chromatography
8. washeluting with petroleum ether/ethyl acetate (from 4:1 to 1:2)