HRID1861874

反应详情

EQUATION

反应方程式

HRID 1861874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

CuCN (2.01 g, 22.40 mmol) is introduced into a round-bottomed flask placed under argon, THF (60 ml) is then added and the mixture is cooled to −78° C. n-Butyl-lithium (1.6 M, 27.7 ml, 44.40 mmol) is then added drop-wise and the mixture is allowed to slowly return to room temperature. It is again cooled to −78° C. and n-Bu3SnH (12 ml, 44.40 mmol) is added and the mixture is stirred for 10 minutes, during which the hydrogen is discharged. (2E)-3-Methylpent-2-en-4-yn-1-ol (1.86 g, 19.31 mmol) is then added, the reaction mixture is left stirring for 45 minutes and then poured into 200 ml of an NH4OH/NH4Cl (10/90) solution. Extraction is carried out with ether (3×100 ml), drying is carried out over Na2SO4 and evaporation is carried out under vacuum.

WORKUP

后处理

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  2. customto slowly return to room temperature
  3. waitthe reaction mixture is left
  4. extractionExtraction
  5. customdrying
  6. customis carried out over Na2SO4 and evaporation