反应详情

温度

50 °C

A mixture of (E)-dimethyl 2-(2-fluoro-3-methylphenylimino)succinate (7-14, 14.59 g, 54.6 mmol) and Eaton's reagent (52.0 mL, 328 mmol) was heated at 50° C. for 1 h. After cooling to room temperature, the mixture was added slowly to a cold sat. NaHCO3 solution (gas released!), followed by EtOAc extraction (twice). The combined organic fractions were washed with brine, dried (Na2SO4), filtered and the solvent was evaporated under reduced pressure to afford methyl 8-fluoro-4-hydroxy-7-methylquinoline-2-carboxylate (7-15, 11.9 g). LRMS m/z (M+H)+ 236.2 found, 236.1 required.

1. temperatureAfter cooling to room temperature
2. extractionfollowed by EtOAc extraction (twice)
3. washThe combined organic fractions were washed with brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customthe solvent was evaporated under reduced pressure