反应详情

温度

110 °C

3-Bromo-6-methoxycatechol (23.4 g) was dissolved in DMF (150 ml), and dibromomethane (15.4 ml) and potassium fluoride (31.1 g) were added thereto, followed by heating at 110° C. for 6 hours with stirring. After being allowed to stand for cooling, water was added to the mixture followed by extraction with ether. The organic layer was washed with an aqueous solution of sodium hydroxide, with water, and with a saturated saline, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/1) to give Compound IIbj-a (5.6 g, 40%) as a white solid.

1. temperaturefor cooling
2. extractionfollowed by extraction with ether
3. washThe organic layer was washed with an aqueous solution of sodium hydroxide, with water
4. dry with materialwith a saturated saline, and dried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/1)
7. customto give Compound IIbj-a (5.6 g, 40%) as a white solid