HRID394654
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter 18 hours of reflux under an inert atmosphere
- temperaturethe mixture is cooled
- extractionThe aqueous phase is extracted with dichloromethane
- washthe organic phase is then washed several times with a saturated solution of sodium hydrogen carbonate
- dry with materialAfter drying over magnesium sulphate and evaporation of the solvent in vacuo
- customthe residue obtained
- customis purified on a silica column (eluant: AcOEt/PE: 30/70)