HRID1881399
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Benzyl 4,4,4-trifluoro-3-methylbut-2-enoate (1.87 g, 7.67 mmol) in diethyl ether (5 mL) was added dropwise to a suspension of LAH (291 mg, 1.67 mmol) in diethyl ether (10 mL). After stirring at −78° C. for 10 min and at 0° C. for a further 30 min, the reaction mixture was filtered through cotton, quenched with sodium potassium tartrate and stirred vigorously until layers separated. The aqueous phase was extracted with diethyl ether. The combined ethereal layers were dried (magnesium sulfate) and concentrated in vacuo to afford 4,4,4-trifluoro-3-methylbut-2-en-1-ol which was used in the subsequent step without further purification.
WORKUP
后处理
- filtrationthe reaction mixture was filtered through cotton
- customquenched with sodium potassium tartrate
- stirringstirred vigorously until layers
- customseparated
- extractionThe aqueous phase was extracted with diethyl ether
- dry with materialThe combined ethereal layers were dried (magnesium sulfate)
- concentrationconcentrated in vacuo