反应 #2271684

反应方程式

3,5-dibromo-4-hydroxyacetophenone

K2CO3

1,3-dibromopropane

→

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

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度at reflux 5 hours
2. 2
   其他The solvent was removed
3. 3
   萃取The crude product was extracted into dichloromethane (150 ml)
4. 4
   过滤the insoluble inorganics were filtered off
5. 5
   浓缩The solution was concentrated to dryness again
6. 6
   其他Purification
7. 7
   其他The material thus obtained (2.8 g)
8. 8
   其他was recrystallized twice from isopropyl ether

实验过程

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.

来源