HRID1665822
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 (558 mg, 1.67 mmol) prepared in Example 6 was dissolved in dried pyridine (8 mL). To the solution was added 4,4′-dimethoxytrityl chloride (622 mg, 1.84 mmol), followed by stirring at room temperature. The reaction system was concentrated under reduced pressure, diluted with ethyl acetate, and then washed with a saturated sodium hydrogen carbonate aqueous solution. The organic layer was dried with anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography eluting with chloroform:methanol (98:2, v/v) containing 0.5% triethylamine to give the title compound (749 mg, 70%).
WORKUP
后处理
- concentrationThe reaction system was concentrated under reduced pressure
- additiondiluted with ethyl acetate
- washwashed with a saturated sodium hydrogen carbonate aqueous solution
- dry with materialThe organic layer was dried with anhydrous sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure
- washeluting with chloroform:methanol (98:2
- additionv/v) containing 0.5% triethylamine