反应详情

A suspension of ethyl 4-ethyl-7-fluoro-6-methoxy-2-oxo-1,2-dihydro-3-quinolinecarboxylate (19.4 g, 0.066 mol) in phosphoryl chloride (243 ml) is heated at reflux for 6 hours. The phosphoryl chloride is distilled off. The reaction mixture is decanted into ice-cooled water, then taken up in dichloromethane to solubilize. The organic phase is washed with water, then with a saturated solution of sodium chloride. The organic phase is dried over magnesium sulphate and the solvent is evaporated off. The residue is suspended in ether and the non-converted starting product (4 g) is filtered out. The filtrate is evaporated and the residue is purified by column chromatography (SiO2, AcOEt/Hpt: 5/95 to 20/80). 10.9 g of a white solid is obtained.

1. temperatureis heated
2. temperatureat reflux for 6 hours
3. distillationThe phosphoryl chloride is distilled off
4. customThe reaction mixture is decanted into ice-
5. temperaturecooled water
6. washThe organic phase is washed with water
7. dry with materialThe organic phase is dried over magnesium sulphate
8. customthe solvent is evaporated off
9. filtrationthe non-converted starting product (4 g) is filtered out
10. customThe filtrate is evaporated
11. customthe residue is purified by column chromatography (SiO2, AcOEt/Hpt: 5/95 to 20/80)