反应详情

Cs2CO3 (4.1 g, 12.6 mmol) and 4A sieves were dried under high vacuum at 150° C. for 6 to 10 hours before the start of the reaction. After cooling to room temperature, compound 94A (0.736 g, 2.53 mmol) and compound 1B (1.62 g, 3 mmol) were transferred to the reaction vessel and the atmosphere was purged with nitrogen. 12 mL of anhydrous DMA were then added and the reaction was stirred at 120° C. for 12 hours. The cooled reaction mixture was then diluted with ethyl acetate and 10% citric acid. The organic phase was washed three times with citric acid, once with water and brine, and dried over Na2SO4. Concentration afforded an orange film/foam. Purification on Flash Master (SiO2, ethyl acetate/petroleum ether 0:100 to 40:60) afforded a white solid (1.15 g, 80% yield): 1H NMR (300 MHz, DMSO-d6) δ ppm 12.84 (1H, s), 8.03 (1H, d), 7.77 (2H, m), 7.58 (1H, d), 7.40 (4H, m), 6.86 (1H, d), 4.92 (2H, s), 3.78 (2H, t), 3.01 (2H, t), 1.34 (9H, s).

1. customthe atmosphere was purged with nitrogen
2. addition12 mL of anhydrous DMA were then added
3. customThe cooled reaction mixture
4. washThe organic phase was washed three times with citric acid
5. dry with materialonce with water and brine, and dried over Na2SO4
6. concentrationConcentration
7. customafforded an orange film/foam
8. customPurification on Flash Master (SiO2, ethyl acetate/petroleum ether 0:100 to 40:60)