反应详情

温度

-5 °C

In a flask equipped with a stirrer, a thermometer and a dropping funnel, 3.36 g of sodium hydride was dissolved in 50 ml of THF under nitrogen atmosphere and the solution was cooled down to −5° C. with stirring. 30 ml of a THF solution of ethyl diethylphosphinoacetate (18.8 g) was added dropwise thereto, and the solution was further stirred for 2 hours. After observing hydrogen gas generation, 50 ml of a THF solution of trans-4-(trans-4-propylcyclohexyl)-cyclohexanecarbaldehyde (16.5 g) was added dropwise. Further, the solution was warmed to room temperature and stirred for 3 hours. After stirring, water was added to the reaction mixture and extracted with toluene (50 ml×3). The organic layer was washed with water, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain 10.0 g of ethyl 3-(trans-4-(trans-4-propylcyclohexyl)cyclohexyl)propenoate.

1. customIn a flask equipped with a stirrer
2. stirringthe solution was further stirred for 2 hours
3. additionwas added dropwise
4. temperatureFurther, the solution was warmed to room temperature
5. stirringstirred for 3 hours
6. stirringAfter stirring
7. extractionextracted with toluene (50 ml×3)
8. washThe organic layer was washed with water
9. dry with materialdried over anhydrous magnesium sulfate
10. concentrationconcentrated under reduced pressure