反应详情

温度

80 °C

2,3,4-trimethoxybenzoic acid (7.3 g) was dissolved in methanol (73 ml), mixed with sulfuric acid (15 ml), and stirred for 3 hours while heating at 80° C. The resultant was allowed to stand for cooling, evaporated under reduced pressure for removing the solvent, and the residue was added to cold water, followed by extraction with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate water and then with a saturated aqueous sodium chloride solution, dried over sodium sulfate anhydride, and evaporated under reduced pressure for removing the solvent to give Compound IIbt-a (6.8 g, 87%) as a colorless oily substance.

1. temperaturefor cooling
2. customevaporated under reduced pressure
3. customfor removing the solvent
4. additionthe residue was added to cold water
5. extractionfollowed by extraction with ethyl acetate
6. washThe organic layer was washed with saturated sodium bicarbonate water
7. dry with materialwith a saturated aqueous sodium chloride solution, dried over sodium sulfate anhydride
8. customevaporated under reduced pressure
9. customfor removing the solvent
10. customto give Compound IIbt-a (6.8 g, 87%) as a colorless oily substance