反应详情

To a magnetically stirred solution of 2-bromo-1-(4-methoxy-phenyl)-ethanone (3.0 g, 13.09 mmol) and 5-methyl-pyridin-2-ylamine (1.42 g, 13.09 mmol) in EtOH (30 mL) under Ar atmosphere was added sodium carbonate (2.77 g, 26.18 mmol). The reaction mixture was refluxed for 4 h. The mixture was cooled to room temperature and concentrated in vacuo. Water (60 mL) was added, and the aqueous phase was extracted with dichloromethane (100 mL). The combined organic layers were washed with water (100 mL), dried (MgSO4), and concentrated in vacuo to provide the title compound (2.8 g, 90%) as a white solid. 1H NMR (400 MHz, CDCl3) δ 2.27 (s, 3H), 3.82 (s, 3H), 6.95 (m, 3H), 7.48 (d, J=8.8 Hz, 1H), 7.65 (s, 1H), 7.85 (m, 3H).

1. temperatureThe reaction mixture was refluxed for 4 h
2. concentrationconcentrated in vacuo
3. additionWater (60 mL) was added
4. extractionthe aqueous phase was extracted with dichloromethane (100 mL)
5. washThe combined organic layers were washed with water (100 mL)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo