HRID1043178
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 methyl 4-fluoro-2-hydroxybenzoate (1.225 g) in anhydrous tetrahydrofuran (25 mL) was added potassium t-butoxide (0.808 g). The mixture was stirred for 20 minutes at room temperature. A solution of 1,3-difluoro-2-nitrobenzene (0.955 g) in tetrahydrofuran (6 mL) was then added dropwise. The resulting mixture was stirred at room temperature for 1 hour, then at 80° C. overnight. The reaction mixture was quenched with water (40 mL) and extracted with dichloromethane. The organic solution was dried (MgSO4), filtered and concentrated. The residue was purified on a silica gel column, eluting with 25% ethyl acetate in hexane to obtain the title compound.
WORKUP
后处理
- stirringThe resulting mixture was stirred at room temperature for 1 hour
- customat 80° C.
- customovernight
- customThe reaction mixture was quenched with water (40 mL)
- extractionextracted with dichloromethane
- dry with materialThe organic solution was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified on a silica gel column
- washeluting with 25% ethyl acetate in hexane