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 (83.8 mg) obtained in Example 19-3 was dissolved in anhydrous dichloromethane (1.5 ml). The solution was added with triethylamine (70.1 μl) and then added with n-heptyl chloroformate (74.9 μl) in an ice bath, followed by stirring overnight under a nitrogen atmosphere at room temperature. After completion of the reaction, the solution was added with a saturated aqueous sodium bicarbonate solution and stirred for a while. Then, the solution was extracted with chloroform and washed with a saturated aqueous sodium bicarbonate solution and saturated saline solution. The organic layer was dried with anhydrous sodium sulfate. Subsequently, the solvent was distilled off and the residue was then purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (111 mg) as a brown solid.
WORKUP
后处理
- customAfter completion of the reaction
- stirringstirred for a while
- extractionThen, the solution was extracted with chloroform
- washwashed with a saturated aqueous sodium bicarbonate solution and saturated saline solution
- dry with materialThe organic layer was dried with anhydrous sodium sulfate
- distillationSubsequently, the solvent was distilled off
- customthe residue was then purified through silica gel column chromatography (chloroform/methanol)