HRID2361286
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 solution of 6-fluoroisobenzofuran-1(3H)-one (0.549 g, 3.61 mmol) in methanol (12 mL) and water (3 mL) at room temperature was added potassium hydroxide (0.350 g, 6.24 mmol). The mixture was heated at reflux for 1.5 hr. The mixture was concentrated under vacuum to a volume of about 3 mL. The residue was acidified with 1 M KHSO4 solution to pH 3-4. The insoluble material (inorganic salt) was removed by suction filtration and the filtrate was extracted with ethyl acetate (5×30 mL). The combined extract was dried over anhydrous MgSO4. Removal of solvent under vacuum provided the desired product (0.479 g, 2.82 mmol, 78% yield) as a white solid.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux for 1.5 hr
- concentrationThe mixture was concentrated under vacuum to a volume of about 3 mL
- customThe insoluble material (inorganic salt) was removed by suction filtration
- extractionthe filtrate was extracted with ethyl acetate (5×30 mL)
- extractionThe combined extract
- dry with materialwas dried over anhydrous MgSO4
- customRemoval of solvent under vacuum