反应详情

温度

70 °C

A mixture of 5-bromo-2-methoxyphenol (50.0 g), 2-bromo-3-pentanone (68.1 g), potassium carbonate (52.8 g), and DMF (500 ml) was stirred at 70° C. for 2 hours. After being allowed to stand for cooling, water was added to the mixture followed by extraction with ether. The organic layer was washed with a saturated saline and dried over anhydrous magnesium sulfate, and the solvent was distilled off. The residue was purified by silica gel column chromatography (hexane:chloroform=1:1) to give Compound IIb-a (86.8 g, 94.0%) as a pale-yellow oily substance.

1. temperaturefor cooling
2. extractionfollowed by extraction with ether
3. washThe organic layer was washed with a saturated saline
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off
6. customThe residue was purified by silica gel column chromatography (hexane:chloroform=1:1)
7. customto give Compound IIb-a (86.8 g, 94.0%) as a pale-yellow oily substance