反应详情

To a solution of 2-amino-5-fluoropyridine (1.12 g) in diethyl ether (25 ml) was added ethyl bromopyruvate (1.25 ml). The mixture was stirred for 1 hour. The resultant solid was filtered off, suspended in ethanol and heated at reflux for 4 hrs. The solvent was removed by evaporation and the residue partitioned between ethyl acetate (100 ml) and aqueous sodium bicarbonate solution (100 ml). The organic layer was separated, dried with MgSO4, and the solvent removed by evaporation. The residue was purified by flash chromatography (silica) eluting with ethyl acetate:hexane (3:1) to give the sub-title compound as a colourless solid (1.12 g).

1. filtrationThe resultant solid was filtered off
2. temperatureheated
3. temperatureat reflux for 4 hrs
4. customThe solvent was removed by evaporation
5. customthe residue partitioned between ethyl acetate (100 ml) and aqueous sodium bicarbonate solution (100 ml)
6. customThe organic layer was separated
7. dry with materialdried with MgSO4
8. customthe solvent removed by evaporation
9. customThe residue was purified by flash chromatography (silica)
10. washeluting with ethyl acetate:hexane (3:1)