HRID478071
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
To a stirred solution of lithium diisopropylamide (LDA) (22 mmol) in THF (200 ml) at -78° C. was added a solution of 2,3-dimethylcyclohexenone (2.48 g, 20 mmol) in THF (50 ml). The mixture was warmed to 25° C., and the solvent and the amine were removed under vacuum. The resulting solid was dissolved in THF (400 ml) and the solution cooled to -78° C. To this solution was added MVK (1.8 ml, 22 mmol) in THF (100 ml) over 10 min. The resulting mixture was stirred 12 hr at room temperature, then worked up. Removal of solvent yielded the dione as a yellow oil (2.8 g, 60%).
WORKUP
后处理
- customthe solvent and the amine were removed under vacuum
- dissolutionThe resulting solid was dissolved in THF (400 ml)
- temperaturethe solution cooled to -78° C
- additionTo this solution was added MVK (1.8 ml, 22 mmol) in THF (100 ml) over 10 min
- customRemoval of solvent