反应 #324687

反应方程式

2-(4-Bromo-3,5-dimethyl-phenoxy)-2-methyl-propionic acid

HCl water

→

title compound

2-(4-Bromo-3,5-dimethyl-phenoxy)-2-methyl-propan-1-ol

溶剂

tetrahydrofurane

反应条件

后处理

1. 1
   workup.ADDITIONborane methylsulfide complex (2.6 mL) is added
2. 2
   温度The reaction mixture is cooled to 0° C.
3. 3
   萃取the reaction mixture is extracted with dichloromethane
4. 4
   其他The organic phase is separated
5. 5
   干燥dried over sodium sulfate
6. 6
   浓缩concentrated under vacuum
7. 7
   其他The residue is chromatographed on silica gel (hexane/ethyl acetate 100:0→50:50)

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.

来源