反应详情

In N,N-dimethylformamide (15 ml) was dissolved 7-methoxy-4-methylquinolin-2(1H)one (1.5 g, 6.06 mmol), sodium iodide (2.3 g, 15.9 mmol) was added thereto under cooling on ice and lithium hydride (188 mg, 15.9 mmol) was gradually added thereto. After stirring for 1 hour under cooling on ice, 2-(2-bromoethyl)-1,3-dioxolane (1.6 ml, 15.9 mmol) was gradually added thereto. The reaction solution was stirred overnight at room temperature and then the extract was partitioned into ethyl acetate-water, whereby the organic layer was separated. The obtained organic layer was washed with water and saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to yield 1 g (57%) of the title compound.

1. additionwas added
2. additionwas gradually added
3. additionwas gradually added
4. stirringThe reaction solution was stirred overnight at room temperature
5. customthe extract was partitioned into ethyl acetate-water, whereby the organic layer
6. customwas separated
7. washThe obtained organic layer was washed with water and saturated sodium chloride solution
8. dry with materialdried over anhydrous sodium sulfate
9. customThe solvent was removed under reduced pressure
10. customthe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)