HRID1443598

反应详情

EQUATION

反应方程式

HRID 1443598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 ml of a 15% solution of Dess-Martin periodinane=1,1,1-tris(acetyloxy)-1,1-di-hydro-1,2-benziodoxol-3-(1H)-one in dichloromethane was added dropwise to 1.5 g of 2-(5-hydroxypentyl)-2-(3,3,3-trifluoropropyl)malononitrile, and the mixture was stirred at room temperature for 5 hours. Thereafter, the reaction mixture was added to an aqueous dilute sodium hydroxide solution and then extracted with chloroform. The organic layer was washed successively with water and aqueous sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 1.0 g of 2-(5-oxopentyl)-2-(3,3,3-trifluoropropyl)malononitrile.

WORKUP

后处理

  1. extractionextracted with chloroform
  2. washThe organic layer was washed successively with water and aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure