反应详情

温度

85 °C

2-(2-bromo-4-fluoro-5-nitrophenyl)acetic acid (6.04 g, 21.7 mmol) and cone. H2SO4 (1.2 mL) were combined in EtOH (100 mL) and stirred with heating at 85° C. After 1.5 h, the completed reaction was cooled to RT and concentrated as completely as possible. The residue was dissolved in MTBE (50 mL) and washed with H2O (2×), and brine (2×), dried (MgSO4), filtered and evaporated to afford a dark orange oil. The crude was purified by silica gel column chromatography to obtain ethyl 2-(2-bromo-4-fluoro-5-nitrophenyl)acetate (5.8 g, 87% yield).

1. customthe completed reaction
2. temperaturewas cooled to RT
3. concentrationconcentrated as completely as possible
4. dissolutionThe residue was dissolved in MTBE (50 mL)
5. washwashed with H2O (2×), and brine (2×)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customevaporated
9. customto afford a dark orange oil
10. customThe crude was purified by silica gel column chromatography