反应详情

A mixture of 2-amino-6-fluorophenol (2 g, 8.3 mmol), of ethyl 2,3-dibromopropionate (1.46 mL, 9.96 mmol) and of K2CO3 (3.44 g, 24.9 mmol) in acetone (80 mL) is heated under reflux for 9 h 15 min. The mixture is cooled and filtered. The filtrate is vacuum concentrated, the residue dissolved in iced aqueous NaOH solution (1N, 10 mL) and extracted with ethyl ether. The ethereal phase is washed in water then saline water, dried over MgSO4 and concentrated under reduced pressure. The residue is purified by filtering though silica gel using dichoromethane as eluting solvent. The title compound is obtained in oil form (1.1 g, 59%).

1. temperatureunder reflux for 9 h 15 min
2. temperatureThe mixture is cooled
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionthe residue dissolved in iced aqueous NaOH solution (1N, 10 mL)
6. extractionextracted with ethyl ether
7. washThe ethereal phase is washed in water
8. dry with materialdried over MgSO4
9. concentrationconcentrated under reduced pressure
10. customThe residue is purified
11. filtrationby filtering though silica gel
12. washas eluting solvent