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
In an argon atmosphere, 4-[4-(1H-1,2,3-triazol-1-yl)butyl]phenol (218 mg) and 65% oily sodium hydride (39 mg) were dissolved in DMF (5 ml) added thereto. With stirring under ice cooling, 4-(chloromethyl)-2-[(E)-2-(4-fluorophenyl)ethenyl]-1,3-oxazole (250 mg) was added, followed by stirring at room temperature for 3 hours. After water was added, the reaction mixture was extracted with ethyl acetate. The extract was washed with water and saturated saline and dried over sodium sulfate, after which it was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform-ethanol=24:1), after which it was recrystallized from ethyl acetate to yield the titled compound (368 mg) as colorless crystals.
WORKUP
后处理
- additionadded
- stirringby stirring at room temperature for 3 hours
- extractionthe reaction mixture was extracted with ethyl acetate
- washThe extract was washed with water and saturated saline
- dry with materialdried over sodium sulfate
- concentrationafter which it was concentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (eluent: chloroform-ethanol=24:1)
- customafter which it was recrystallized from ethyl acetate