HRID433067
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Under an argon atmosphere, 0.56 mmol of the compound obtained in Step A are dissolved in 5 ml of DMF, and then 0.68 mmol of NaH are added at 0° C., over a period of 30 minutes. After 30 minutes' stirring at 0° C., 0.68 mmol of 2-iodobenzoyl chloride dissolved in 5 ml of DMF is added dropwise to the mixture. After 3 hours' stirring, the solvents are removed by evaporation and the residue is taken up in water and extracted with dichloromethane. After drying over magnesium sulphate and removal of the solvents by evaporation, the residue is purified by flash chromatography over silica gel (eluant:petroleum ether/ethyl acetate) to yield the title compound.
WORKUP
后处理
- additionis added dropwise to the mixture
- stirringAfter 3 hours' stirring
- customthe solvents are removed by evaporation
- extractionextracted with dichloromethane
- dry with materialAfter drying over magnesium sulphate and removal of the solvents by evaporation
- customthe residue is purified by flash chromatography over silica gel (eluant:petroleum ether/ethyl acetate)