HRID1090561
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
310 mg of the amorphous compound obtained in Example 6 was dissolved in 2 ml of 1,2-ethanedithiol, and to the solution were added 1 ml of boron trifluoride/ethyl ether, and after stirring at a room temperature for 18 hours, was added saturated sodium bicarbonate aqueous solution, and the reaction mixture was extracted twice with a mixture of chloroform and methanol (10:1). The extract was dried over magnesium sulfate, and concentrated under a reduced pressure to obtain a residue, which was applied to a silica gel column and eluted with chloroform/methanol (80:1 to 20:1) to obtain 148 mg of the title compound in a colorless amorphous form.
WORKUP
后处理
- extractionthe reaction mixture was extracted twice with a mixture of chloroform and methanol (10:1)
- dry with materialThe extract was dried over magnesium sulfate
- concentrationconcentrated under a reduced pressure
- customto obtain a residue, which
- washeluted with chloroform/methanol (80:1 to 20:1)