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 (613 mg) obtained in Example 29-4 was dissolved in THF (18 ml) and added with 60% sodium hydride (105 mg). After that, the whole was gradually added with methyl iodide (373 mg) and stirred at room temperature for 16 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform, washed with water, and subjected to extraction with chloroform. The organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off. The residue was purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (160 mg) as a brown solid.
WORKUP
后处理
- customAfter completion of the reaction
- distillationthe solvent was distilled off under reduced pressure
- dissolutionThe residue was dissolved in chloroform
- washwashed with water
- extractionsubjected to extraction with chloroform
- washThe organic layer was washed with a saturated saline solution
- dry with materialdried with anhydrous sodium sulfate
- filtrationAfter filtration
- distillationthe solvent was distilled off
- customThe residue was purified through silica gel column chromatography (hexane/ethyl acetate)