反应详情

To a stirring solution of 1 (2.0 g, 10.75 mmol) and K2CO3 (2.96 g, 21.5 mmol) in dry DMF (20 mL) was added 2 (1.59 g, 10.75 mmol) and the reaction mixture was stirred at rt for 16 h under nitrogen atmosphere. It was cooled, quenched with water (100 mL) and extracted with EtOAc (2×50 mL). The combined EtOAc extract was washed with 10% NaHCO3 soln. (50 mL), water (3×50 mL), brine (50 mL), dried over Na2SO4 and concentrated under reduced pressure to give 3 (1.92 g, 60.0%) as a light yellow solid, which was used in the next step without further purifications.

1. temperatureIt was cooled
2. customquenched with water (100 mL)
3. extractionextracted with EtOAc (2×50 mL)
4. extractionThe combined EtOAc extract
5. washwas washed with 10% NaHCO3 soln
6. dry with material(50 mL), water (3×50 mL), brine (50 mL), dried over Na2SO4
7. concentrationconcentrated under reduced pressure