HRID1443595

反应详情

EQUATION

反应方程式

HRID 1443595 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.5 g of 2-(3,3,3-trifluoropropyl)malononitrile, 5.5 g of 5-bromopentyl benzyl ether and 0.70 g of potassium iodide were dissolved in 20 ml of dimethyl sulfoxide, 3.3 g of potassium carbonate was added, and the mixture was stirred at room temperature for 9 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 5.9 g of 2-(5-benzyloxypentyl)-2-(3,3,3-trifluoropropyl)malononitrile.

WORKUP

后处理

  1. extractionfollowed by extraction with methyl tert-butyl ether
  2. washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure