HRID1587185
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
216 mg of the amorphous compound obtained in Example 32 was dissolved in 3 ml of methanol, and to the solution was added 0.6 ml of 2 N potassium hydroxide aqueous solution. The mixture was refluxed for 10 hours, and after the addition of 30 ml of saturated sodium chloride aqueous solution, extracted twice with 20 ml of a mixed solvent of chloroform/isopropanol (5:1). The extract was dried over magnesium sulfate and concentrated under a reduced pressure, and a resulting residue was applied to a silica gel column and eluted with chloroform/methanol (40:1 to 10:1) to obtain 74 mg of the title compound in a colorless amorphous form.
WORKUP
后处理
- temperatureThe mixture was refluxed for 10 hours
- extractionextracted twice with 20 ml of a mixed solvent of chloroform/isopropanol (5:1)
- dry with materialThe extract was dried over magnesium sulfate
- concentrationconcentrated under a reduced pressure
- washeluted with chloroform/methanol (40:1 to 10:1)