反应详情

温度

75 °C

To the product of Step C (0.500 g, 1.465 mmol) was added Ag2CO3 (0.606 g, 2.198 mmol), DMF (8 mL), and 3,4-difluorobenzyl bromide (0.28 mL, 2.198 mmol). The reaction was heated to 75° C. for 75 min before cooling and filtering through Celite®545 diatomaceous earth. The solution was concentrated and the residue was purified by flash chromatography (silica gel) eluting with a gradient of 15 to 46% ethyl acetate/hexane affording the product. MS (electrospray) m/e 467.0 MH+ (Rt=4.7 min LC/MS).

1. temperaturebefore cooling
2. filtrationfiltering through Celite®545 diatomaceous earth
3. concentrationThe solution was concentrated
4. customthe residue was purified by flash chromatography (silica gel)
5. washeluting with a gradient of 15 to 46% ethyl acetate/hexane affording the product