反应详情

温度

80 °C

Anhydrous potassium carbonate (6.71 g, 48 mmol) was added to a solution of Example 154a (3.9 g, 9.7 mmol) in DMF (200 ml) and the reaction mixture was stirred at 80° C. for 4.5 h. It was concentrated and treated with ethyl acetate, then washed with 10% aqueous HCl, water, brine, dried, concentrated and purified using flash chromatography (silica gel, ethyl acetate/pet ether) to obtain the title compound as a white solid. Yield: 1.2 g (40%); 1H NMR (CDCl3): δ 2.64 (s, 3H, CH3), 3.88 (s, 3H, OCH3), 4.2 (s, 2H, CH2), 7.08 (m, 2H, Ar), 7.32 (q, 1H, Ar), 7.6 (s, 1H, Ar), 7.65 (s, 1H, Ar); MS: m/e (EI+) 320 (M+).

1. concentrationIt was concentrated
2. additiontreated with ethyl acetate
3. washwashed with 10% aqueous HCl, water, brine
4. customdried
5. concentrationconcentrated
6. custompurified