反应详情

温度

80 °C

To a stirred solution of 2 (4.35 g, 23.38 mmol) and Cs2CO3 (15.26 g, 46.76 mmol) in dry DMF (50 mL) was added 1 (5.0 g, 15.58 mmol) at rt and the reaction was stirred at 80° C. for 16 h under nitrogen atmosphere. The reaction mixture was cooled, concentrated under reduced pressure and the residue was diluted with ethyl acetate (50 mL). It was washed with water (2×10 mL), brine (10 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue was further purified by column chromatography (SiO2, 60-120, pet ether/ethyl acetate, 5/5) to give 3 (1.6 g, 23.3%) as brown solid.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated under reduced pressure
3. additionthe residue was diluted with ethyl acetate (50 mL)
4. washIt was washed with water (2×10 mL), brine (10 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customThe residue was further purified by column chromatography (SiO2, 60-120, pet ether/ethyl acetate, 5/5)