HRID1847109
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
Compound 1 (400 mg, 0.999 mmol) obtained in Example 1 was dissolved in a mixed solvent of methanol (6.0 mL) and dichloromethane (4.0 mL), and sodium borohydride (37.8 mg, 0.999 mmol) was added thereto at 0° C., followed by stirring at 20 minutes. A saturated aqueous ammonium chloride solution was added to the reaction mixture, followed by extraction with ethyl acetate twice. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to yield a residue. The residue was purified by silica gel column chromatography to obtain the title compound (363 mg, 90%).
WORKUP
后处理
- additionwas added
- customat 0° C.
- extractionfollowed by extraction with ethyl acetate twice
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto yield a residue
- customThe residue was purified by silica gel column chromatography