HRID1110417

反应详情

EQUATION

反应方程式

HRID 1110417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.22 g (10 mmol) of salicylaldehyde together with 0.66 g (10 mmol) of 3-oxo-1-butene are added at room temperature to a suspension of 0.14 g (1 mmol) of potassium carbonate in 50 ml of 2™butanone. The mixture is brought to reflux with stirring and this temperature is maintained for 4 hours. The reaction medium is evaporated on a water bath under vacuum and the residue taken up with 100 ml of water and extracted three times with 75 ml of diethyl ether. The organic phases are combined, washed to neutrality with saturated aqueous sodium chloride solution, dried over sodium sulfate and filtered, the filtrate is evaporated on a water bath under vacuum and the product recrystallized in hexane

WORKUP

后处理

  1. temperatureto reflux
  2. temperaturethis temperature is maintained for 4 hours
  3. customThe reaction medium is evaporated on a water bath under vacuum
  4. extractionextracted three times with 75 ml of diethyl ether
  5. washwashed to neutrality with saturated aqueous sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customthe filtrate is evaporated on a water bath under vacuum
  9. customthe product recrystallized in hexane