HRID394654

反应详情

EQUATION

反应方程式

HRID 394654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4 g (16 mmol) of the ester obtained in Step C are dissolved in 60 ml of anhydrous dichloromethane; 6.1 g (35.4 mmol) of meta-chloroperbenzoic acid are then added to the medium. After 18 hours of reflux under an inert atmosphere, the mixture is cooled and then hydrolysed with ice-cold water. The aqueous phase is extracted with dichloromethane; the organic phase is then washed several times with a saturated solution of sodium hydrogen carbonate. After drying over magnesium sulphate and evaporation of the solvent in vacuo, the residue obtained is purified on a silica column (eluant: AcOEt/PE: 30/70) to yield the title ester in the form of a syrup.

WORKUP

后处理

  1. temperatureAfter 18 hours of reflux under an inert atmosphere
  2. temperaturethe mixture is cooled
  3. extractionThe aqueous phase is extracted with dichloromethane
  4. washthe organic phase is then washed several times with a saturated solution of sodium hydrogen carbonate
  5. dry with materialAfter drying over magnesium sulphate and evaporation of the solvent in vacuo
  6. customthe residue obtained
  7. customis purified on a silica column (eluant: AcOEt/PE: 30/70)