HRID1171211
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To an ethanol (5 mL) solution of 2-(6-phenoxy-benzofuran-2-ylmethyl)-isoindole-1,3-dione (209 mg, 566 μmol) described in Production Example 49-1-3 was added hydrazine hydrate (549 μL, 11.3 mmol) at room temperature, which was stirred for 1 hour while heating under reflux. Water was added to the reaction solution at room temperature followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under a reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate:methanol=10:1) to obtain the title compound (92 mg, 68%) as a colorless oil.
WORKUP
后处理
- temperaturewhile heating
- temperatureunder reflux
- extractionfollowed by extraction with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated under a reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate:methanol=10:1)