HRID478071

反应详情

EQUATION

反应方程式

HRID 478071 的结构方程式

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

  1. customthe solvent and the amine were removed under vacuum
  2. dissolutionThe resulting solid was dissolved in THF (400 ml)
  3. temperaturethe solution cooled to -78° C
  4. additionTo this solution was added MVK (1.8 ml, 22 mmol) in THF (100 ml) over 10 min
  5. customRemoval of solvent