HRID216353

反应详情

EQUATION

反应方程式

HRID 216353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationthe reaction mixture was filtered through cotton
  2. customquenched with sodium potassium tartrate
  3. stirringstirred vigorously until layers
  4. customseparated
  5. extractionThe aqueous phase was extracted with diethyl ether
  6. dry with materialThe combined ethereal layers were dried (magnesium sulfate)
  7. concentrationconcentrated in vacuo