HRID1071635

反应详情

EQUATION

反应方程式

HRID 1071635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Methyl-2-(3-thienyl)butanenitrile (6.23 g) obtained using 3-thienylacetonitrile as a starting material in accordance with the method of Example 114 described in JP-A 11-206862 and ethyl acrylate (4.53 g) were dissolved in dimethylformamide (15 ml), and added at a room temperature to a solution of potassium tert-butoxide (423 mg) in dimethylformamide solution (60 ml). After stirring 5 hours as it was, the organic layer was separated by adding an aqueous saturated ammonium chloride and diethyl ether thereto. The resulting organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The drying agent was filtered off, and then the filtrate was evaporated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate system), to give the title compound as a yellow oil (6.66 g, 67%).

WORKUP

后处理

  1. customthe organic layer was separated
  2. additionby adding an aqueous saturated ammonium chloride and diethyl ether
  3. washThe resulting organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe drying agent was filtered off
  6. customthe filtrate was evaporated
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate system)