HRID1861963
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 (1.16 g) obtained in Example 520 was dissolved in methylene chloride (15 ml); to the solution, trifluoroacetic acid (4 ml) was added and the mixture was stirred at room temperature for 1 h. A saturated aqueous sodium bicarbonate solution was added to the reaction mixture, which was extracted with methylene chloride. The organic layer was dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=3:1) to give 480.5 mg of the titled compound (yield, 70%).
WORKUP
后处理
- extractionwas extracted with methylene chloride
- dry with materialThe organic layer was dried with anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=3:1)