反应详情

To a solution of 5-(2-methoxyphenyl)-1,3-cyclohexanedione (2.0 g), acetic acid (0.99 g) and dimethylaminopyridine (1.7 g) in dimethylformamide (100 ml) was added dicyclohexylcarbodiimide (2.5 g), and the mixture was stirred at room temperature for 15 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added ethyl acetate. The solution was washed with potassium hydrogen sulfate solution and water, and to the solution was added 1N sodium hydroxide solution. The aqueous layer was neutralized with 1N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried with magnesium sulfate and concentrated under reduced pressure, and the residue was recrystallized from diisopropylether/hexane to give colorless crystals of 2-acetyl-5-(2-methoxyphenyl)cyclohexane-1,3-dione (2.0 g).

1. customUnder reduced pressure, the solvent was evaporated
2. additionto the residue was added ethyl acetate
3. washThe solution was washed with potassium hydrogen sulfate solution and water
4. additionto the solution was added 1N sodium hydroxide solution
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with water and saturated brine
7. dry with materialdried with magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customthe residue was recrystallized from diisopropylether/hexane