反应详情

温度

50 °C

5-Hydroxy-2-nitrobenzaldehyde dimethyl acetal (3.0 g) is dissolved in dry dimethylformamide (50 ml), and thereto are added sodium iodide (3.15 g), potassium carbonate (1.93 g) and 3-(t-butoxycarbonylamino)propyl tosylate (6.95 g). The mixture is stirred at 50° C. for three hours, and cooled to room temperature. The mixture is extracted with ethyl acetate, and the extract is washed with a saturated aqueous sodium chloride solution, and dried over sodium sulfate. The resultant is concentrated under reduced pressure to remove the solvent, and the residue is purified by silica gel column chromatography to give the title compound (5.22 g) as a pale yellow oil.

1. temperaturecooled to room temperature
2. extractionThe mixture is extracted with ethyl acetate
3. washthe extract is washed with a saturated aqueous sodium chloride solution
4. dry with materialdried over sodium sulfate
5. concentrationThe resultant is concentrated under reduced pressure
6. customto remove the solvent
7. customthe residue is purified by silica gel column chromatography