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 (520 mg) obtained in Example 23-4 was dissolved in anhydrous DMF (10 ml) and added with diisopropylethylamine (463 μl) and diethyl bromomalonate (340 μl) and the whole was stirred at room temperature for 2 hours. After completion of the reaction, a saturated aqueous sodium hydrogen carbonate solution was added thereto and the whole was stirred for a while. The solution was subjected to extraction with chloroform and washed with a saturated saline solution. The organic layer was dried with anhydrous sodium sulfate. The solvent was distilled off. The residue was purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (421 mg) as a colorless oily substance.
WORKUP
后处理
- customAfter completion of the reaction
- stirringthe whole was stirred for a while
- extractionThe solution was subjected to extraction with chloroform
- washwashed with a saturated saline solution
- dry with materialThe 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)