反应详情

温度

150 °C

To a solution of 2-bromo-5-hydroxybenzaldehyde (62; 5 g, 0.025 mol) in DMF (100 ml) was added (R)-4-(chloromethyl)-2,2-dimethyl-1,3-dioxolane (63; 4.87 g, 0.032 mol) and K2CO3 (7.0 g, 0.05 mol). The resulting reaction mixture was stirred at 150° C. for 10 h, cooled to room temperature, diluted with water, and then extracted with EtOAc. The combined organic layers were dried (Na2SO4) and concentrated under reduced pressure. The resulting residue was purified by chromatography (petroleum ether/EtOAc=10:1 to afford the desired product, namely (S)-2-bromo-5-((2,2-dimethyl-1,3-dioxolan-4-yl)methoxy)benzaldehyde 64 (4.1 g, 56%).

1. customThe resulting reaction mixture
2. temperaturecooled to room temperature
3. extractionextracted with EtOAc
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by chromatography (petroleum ether/EtOAc=10:1