反应详情

温度

60 °C

8-Chloro-7-(2,2-dimethoxy-ethoxy)-2-(4-isopropyl-thiazol-2-yl)-quinolin-4-ol (5.0 g, 12.3 mmol) was dissolved in HOAc (100 mL) and 1.4 N HCl/H2O (50 mL). The reaction mixture was heated to 60° C. with stirring for 2 hrs. After cooled back to room temperature and concentrated, the residue was co-evaporated with toluene (2×50 mL). Then the crude was dissolved in DCM (100 mL) and cooled to 0° C. with stirring. Morphiline (1.6 g, 18.4 mmol) and NaHB(OAc)3 (3.9 g, 18.4 mmol) were added to the reaction mixture. After stirring at room temperature for 1 h, the reaction mixture was washed with sat. NaHCO3, brine and dried by Na2SO4. After concentration, the crude was purified by silica gel chromatography to afford 5.0 g of 8-chloro-2-(4-isopropyl-thiazol-2-yl)-7-(2-morpholin-4-yl-ethoxy)-quinolin-4-ol as a white solid.

1. temperatureAfter cooled back to room temperature
2. concentrationconcentrated
3. dissolutionThen the crude was dissolved in DCM (100 mL)
4. temperaturecooled to 0° C.
5. stirringwith stirring
6. stirringAfter stirring at room temperature for 1 h
7. washthe reaction mixture was washed with sat. NaHCO3, brine
8. dry with materialdried by Na2SO4
9. concentrationAfter concentration
10. customthe crude was purified by silica gel chromatography