反应详情

温度

0 °C

To a solution of 2,4-dimethoxyquinoline (11.5 g, 60.8 mmol) in anhydrous THF was added dropwise n-BuLi (2.5 M in hexane, 48.6 mL, 122 mmol) at 0° C. After stirring for 1.5 h at 0° C., the mixture was added to a solution of ethyl chloroformate in anhydrous THF and stirred at 0° C. for additional 30 min and then at room temperature overnight. The reaction mixture was poured into water and extracted with CH2Cl2. The organic layer was dried over Na2SO4 and concentrated under vacuum. The resulting residue was purified by column chromatography (petroleum ether/EtOAc=50/1) to give ethyl 2,4-dimethoxyquinoline-3-carboxylate (9.6 g, 60%).

1. stirringstirred at 0° C. for additional 30 min
2. customat room temperature
3. customovernight
4. extractionextracted with CH2Cl2
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated under vacuum
7. customThe resulting residue was purified by column chromatography (petroleum ether/EtOAc=50/1)