HRID1353152
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
To a dioxane (15 ml) solution of the compound prepared in Example 10, pyridine (363 μl) and trifluoroacetic acid (423 μl) were added, followed by stirring at room temperature for 1 hour. The reaction mixture was concentrated, and the residue was diluted with ethyl acetate. The diluted solution was washed with 1 N hydrochloric acid, water and a saturated saline in this order, dried with anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to thereby obtain the title compound (533 mg) having the following physical data.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additionthe residue was diluted with ethyl acetate
- washThe diluted solution was washed with 1 N hydrochloric acid, water
- dry with materiala saturated saline in this order, dried with anhydrous magnesium sulfate
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1)