反应详情

温度

90 °C

A mixture of methyl 3-hydroxy-4-methoxy benzoate (19.3 g), 2-bromo-3-pentanone (19.2 ml), potassium carbonate (29.3 g), and DMF (193 ml) was stirred at 90° C. for 2 hours. After being allowed to stand for cooling, water was added to the mixture followed by extraction with toluene. The organic layer was washed with a saturated saline and dried over sodium sulfate, and the solvent was distilled off. The residue was purified by column chromatography (silica gel, hexane:ethyl acetate=3:1) to give Compound IIk-a (25.8 g, 91.5%) as a colorless oily substance.

1. temperaturefor cooling
2. extractionfollowed by extraction with toluene
3. washThe organic layer was washed with a saturated saline
4. dry with materialdried over sodium sulfate
5. distillationthe solvent was distilled off
6. customThe residue was purified by column chromatography (silica gel, hexane:ethyl acetate=3:1)
7. customto give Compound IIk-a (25.8 g, 91.5%) as a colorless oily substance