反应详情

温度

65 °C

Potassium carbonate (0.27 g) and benzyl bromide (0.17 mL) were sequentially added to an N,N-dimethylformamide (2 mL) solution of 7-hydroxy-2,3-dihydrobenzo[1,4]dioxine-6-carbaldehyde (0.23 g), followed by stirring at 65° C. for 2 hours. Benzyl bromide (0.077 mL) was added to the reaction mixture, followed by stirring at 65° C. for 30 minutes. The reaction mixture was cooled to room temperature, and then water and ethyl acetate were added thereto. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 75-60% hexane/ethyl acetate] to obtain 0.32 g of 7-(benzyloxy)-2,3-dihydrobenzo[1,4]dioxine-6-carbaldehyde as a light yellow solid.

1. stirringby stirring at 65° C. for 30 minutes
2. temperatureThe reaction mixture was cooled to room temperature
3. customThe organic layer was separated
4. washwashed with a saturated aqueous solution of sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was evaporated under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography [eluent: 75-60% hexane/ethyl acetate]