반응 #324687

반응 방정식

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

용매

tetrahydrofurane

반응 조건

후처리

1. 1
   workup.ADDITIONborane methylsulfide complex (2.6 mL) is added
2. 2
   온도The reaction mixture is cooled to 0° C.
3. 3
   추출the reaction mixture is extracted with dichloromethane
4. 4
   기타The organic phase is separated
5. 5
   건조dried over sodium sulfate
6. 6
   농축concentrated under vacuum
7. 7
   기타The residue is chromatographed on silica gel (hexane/ethyl acetate 100:0→50:50)

실험 절차

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.

출처