HRID333050
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Ethyl (E)-4,4,5,5,5-pentafluoropent-2-enoate (5.5 g, 25.2 mmol) was suspended in 10% NaOH (14.5 ml) and heated at reflux until a homogenous solution was obtained (40 min). After cooling to room temperature the mixture was washed with diethylether (2×) and acidified under ice-cooling with concentrated sulfuric acid. The mixture was extracted with diethylether (3×), the combined organic phases were washed with water, dried over magnesium sulfate and the solvent removed under reduced pressure. 2.64 g (13.9 mmol, 55%) were obtained. MS (ES) M/z=189.0 [M−H]−.
WORKUP
后处理
- temperatureheated
- temperatureat reflux until a homogenous solution
- customwas obtained (40 min)
- washwas washed with diethylether (2×)
- temperaturecooling with concentrated sulfuric acid
- extractionThe mixture was extracted with diethylether (3×)
- washthe combined organic phases were washed with water
- dry with materialdried over magnesium sulfate
- customthe solvent removed under reduced pressure
- custom2.64 g (13.9 mmol, 55%) were obtained