반응 #1180666

반응 방정식

Compound 87-2

2,2-difluoro-5-(3-hydroxypropyl)-1,3-benzodioxole

triphenylphosphine

N-bromosuccinimide

→

product

수율 89.7%

5-(3-bromopropyl)-2,2-difluoro-1,3-benzodioxole

수율 89.7%

용매

methylene chloride

반응 조건

후처리

1. 1
   온도cooling
2. 2
   온도cooling for 2.5 hr
3. 3
   세척The reaction mixture was washed with water and saturated brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타The solvent was evaporated under reduced pressure
6. 6
   workup.ADDITIONDiethyl ether (100 ml) was added
7. 7
   여과the precipitated triphenylphosphine oxide was filtered off
8. 8
   농축The concentrate of the filtrate
9. 9
   기타was purified by silica gel column chromatography

실험 절차

Compound 87-2 (3.54 g) was dissolved in methylene chloride (30 ml), triphenylphosphine (4.73 g) and N-bromosuccinimide (3.21 g) were added under ice-cooling, and the mixture was stirred under ice-cooling for 2.5 hr. The reaction mixture was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Diethyl ether (100 ml) was added, and the precipitated triphenylphosphine oxide was filtered off. The concentrate of the filtrate was purified by silica gel column chromatography to give the object product (4.10 g) as a colorless oil.

출처