HRID1424122
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 (368 mg, 0.70 mmol) obtained in Example 80-1) and 4 M hydrochloric acid (1,4-dioxane solution, 3 mL) in methanol (6 mL) was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, a 5 M aqueous sodium hydroxide solution (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 (200 mg, 69%) as a colorless solid.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additiona 5 M aqueous sodium hydroxide solution (10 mL) was 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)