反应详情

To a solution of ethyl 3-(3,5-dibromopyridin-4-yl)propanoate (4 g, 11.9 mmol) in THF (60 mL) was slowly added n-BuLi (9.52 mL, 23.8 mmol, 2.5 M in hexane) while keeping the inner temperature below −70° C. After the addition, the reaction mixture was stirred below −65° C. for additional 2 hours. The reaction was quenched with water and then extracted with EtOAc (100 mL×3). The combined organic layers were dried over anhy. Na2SO4, filtered, and concentrated in vacuo. The residue was then purified by column chromatography to afford the title compound (1.2 g, 47.6%) as a solid. MS: MS: 213.7 (M+H+, 1Br).

1. customthe inner temperature below −70° C
2. additionAfter the addition
3. customThe reaction was quenched with water
4. extractionextracted with EtOAc (100 mL×3)
5. customThe combined organic layers were dried over anhy
6. filtrationNa2SO4, filtered
7. concentrationconcentrated in vacuo
8. customThe residue was then purified by column chromatography