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 (15 ml) of methyl 4-[chloro(hydroxyimino)methyl]benzoate (0.425 g) and 1-ethynyl-4-trifluoromethylbenzene (0.534 g) in tetrahydrofuran was added dropwise a solution (10 ml) of triethylamine (0.697 ml) in tetrahydrofuran under an argon atmosphere at 0° C. This mixture was stirred overnight at room temperature and poured into water. The mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated. The residue was recrystallized from hexane-ethyl acetate to give methyl 4-[5-(4-trifluoromethylphenyl)-3-isoxazolyl]benzoate (0.563 g, yield 65%) as colorless needle crystals. melting point: 183–184° C.
WORKUP
后处理
- extractionThe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe residue was recrystallized from hexane-ethyl acetate