반응 #2271684

반응 방정식

3,5-dibromo-4-hydroxyacetophenone

K2CO3

1,3-dibromopropane

→

1-[4-(3-bromopropoxy)-3,5-dibromophenyl]ethanone

용매

acetonitrile

반응 조건

후처리

1. 1
   온도at reflux 5 hours
2. 2
   기타The solvent was removed
3. 3
   추출The crude product was extracted into dichloromethane (150 ml)
4. 4
   여과the insoluble inorganics were filtered off
5. 5
   농축The solution was concentrated to dryness again
6. 6
   기타Purification
7. 7
   기타The material thus obtained (2.8 g)
8. 8
   기타was recrystallized twice from isopropyl ether

실험 절차

A stirred mixture of 3,5-dibromo-4-hydroxyacetophenone (3.0 g, 10.1 mmol). K2CO3 (2.8 g, 20.3 mmol), 1,3-dibromopropane (4.0 g, 19.8 mmol) in acetonitrile (100 ml) was heated at reflux 5 hours. The solvent was removed. The crude product was extracted into dichloromethane (150 ml) and the insoluble inorganics were filtered off. The solution was concentrated to dryness again. Purification was carried out by flash chromatography on silica gel (45 g. SiO2: eluted with 1:1 hexane:dichloromethane). The material thus obtained (2.8 g) was recrystallized twice from isopropyl ether to give analytically pure 1-[4-(3-bromopropoxy)-3,5-dibromophenyl]ethanone, m.p.=87°-88° C.

출처