反応 #2271684

反応方程式

3,5-dibromo-4-hydroxyacetophenone

K2CO3

1,3-dibromopropane

→

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

溶媒

acetonitrile

反応条件

後処理

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

実験手順

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.

出典