反应详情

To a solution of 2-methoxybenzaldehyde (2g) in acetone (20 ml), water (40 ml) and acetic acid (4 ml) were added. Under ice cooling, calcium hypochlorite (5.25 g) was added, and then the mixture was stirred at that temperature for 1 hour and at room temperature for 2 hours. The reaction solution was extracted with methyl tert-butyl ether (20 ml×2), and the organic layer was washed with an aqueous sodium thiosulfate solution, then dried over magnesium sulfate. The solvent was distilled off in vacuo and the obtained residue was purified by slurry in heptane. The precipitated crystals were collected by filtration and dried in vacuo to obtain the title compound in an amount of 2.2 g as a colorless crystal.

1. extractionThe reaction solution was extracted with methyl tert-butyl ether (20 ml×2)
2. washthe organic layer was washed with an aqueous sodium thiosulfate solution
3. dry with materialdried over magnesium sulfate
4. distillationThe solvent was distilled off in vacuo
5. customthe obtained residue was purified by slurry in heptane
6. filtrationThe precipitated crystals were collected by filtration
7. customdried in vacuo