HRID237505
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
2-(4-Bromo-3,5-dimethyl-phenoxy)-2-methyl-propionic acid (4.45 g) is dissolved in 50 mL of tetrahydrofurane, borane methylsulfide complex (2.6 mL) is added and the reaction mixture is stirred at room temperature for 5 h. The reaction mixture is cooled to 0° C., 10% HCl water solution is added dropwise and the reaction mixture is extracted with dichloromethane. The organic phase is separated, dried over sodium sulfate and concentrated under vacuum. The residue is chromatographed on silica gel (hexane/ethyl acetate 100:0→50:50) to give the title compound. Yield: 2.6 g.
WORKUP
后处理
- additionborane methylsulfide complex (2.6 mL) is added
- temperatureThe reaction mixture is cooled to 0° C.
- extractionthe reaction mixture is extracted with dichloromethane
- customThe organic phase is separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated under vacuum
- customThe residue is chromatographed on silica gel (hexane/ethyl acetate 100:0→50:50)