HRID1424111
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
A solution of the compound (297 mg, 0.57 mmol) obtained in Example 73-1) and 4 M hydrochloric acid (1,4-dioxane solution, 2 mL) in methanol (10 mL) was stirred at room temperature for 2 h. The reaction mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogencarbonate (10 mL) was added to the residue, the mixture was extracted with ethyl acetate, and the organic layer was washed with saturated sodium chloride solution and dried with anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by silica gel chromatography (ethyl acetate:methanol=20:80) to obtain the title compound (224 mg, 96%) as a colorless solid.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogencarbonate (10 mL)
- additionwas added to the residue
- extractionthe mixture was extracted with ethyl acetate
- washthe organic layer was washed with saturated sodium chloride solution
- dry with materialdried with anhydrous sodium sulfate
- concentrationAfter concentration under reduced pressure
- customthe residue was purified by silica gel chromatography (ethyl acetate:methanol=20:80)