HRID1733290

反应详情

EQUATION

反应方程式

HRID 1733290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-cyanobenzaldehyde (25 g, 0.19 mol), 2-hydroxyacetophenone (25.9 g. 0.19 mol), 38.1 g (0.1 mol) of borax, 250 ml of ethanol, and 250 ml of H2O was refluxed for four days. When cool the reaction mixture was diluted with H2O and extracted with ethyl acetate. The ethyl acetate was dried over anhydrous Na2SO4, filtered, and evaporated to give a dark, tarry residue. The residue was chromatographed on 1 kg of silica gel, eluting with benzene. From this was isolated 5 g of 3'-cyano flavanone as an oil.

WORKUP

后处理

  1. temperaturewas refluxed for four days
  2. temperatureWhen cool the reaction mixture
  3. extractionextracted with ethyl acetate
  4. dry with materialThe ethyl acetate was dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give a dark, tarry residue
  8. customThe residue was chromatographed on 1 kg of silica gel
  9. washeluting with benzene