反应详情

A mixture of 5-(3,5-dimethoxy-phenyl)-quinoline-8-carboxylic acid (Step 159.2) (2 g), H2SO4 conc. (0.6 mL) and EtOH (100 mL) was stirred at reflux for 30 h, allowed to cool and concentrated. The residue was diluted in EtOAc and a saturated aqueous solution of NaHCO3. The aqueous phase was separated and extracted with EtOAc. The combined organic layers were washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was purified by silica gel column chromatography (Hex/EtOAc, 3:2) to provide 1.77 g of the title compound as a white solid. Title compound: ESI-MS: 338.2 [M+H]+; tR 3.81 min (System 1); TLC: Rf=0.29 (Hex/EtOAc, 3:2).

1. temperatureat reflux for 30 h
2. temperatureto cool
3. concentrationconcentrated
4. additionThe residue was diluted in EtOAc
5. customThe aqueous phase was separated
6. extractionextracted with EtOAc
7. washThe combined organic layers were washed with H2O and brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customThe residue was purified by silica gel column chromatography (Hex/EtOAc, 3:2)