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
The compound (1.18 g) obtained in Example 121-6 was dissolved in anhydrous dichloromethane (25 ml) and added with Dess-Martin periodinane (1.82 g), followed by stirring at room temperature for 2 hours. After completion of the reaction, a sodium thiosulfate aqueous solution and a saturated aqueous sodium bicarbonate solution were added to the solution, and the whole was stirred. Then, the solution was extracted with chloroform and the extract was then washed with an aqueous mixture solution of a sodium thiosulfate aqueous solution and a saturated sodium bicarbonate aqueous solution. Then, the organic layer was dried with anhydrous sodium sulfate and the solvent was distilled off. The residue was purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (981 mg) as a white solid.
WORKUP
后处理
- customAfter completion of the reaction
- stirringthe whole was stirred
- extractionThen, the solution was extracted with chloroform
- washthe extract was then washed with an aqueous mixture solution of a sodium thiosulfate aqueous solution
- dry with materialThen, the organic layer was dried with anhydrous sodium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified through silica gel column chromatography (hexane/ethyl acetate)