تفاعل #2271684

معادلة التفاعل

3,5-dibromo-4-hydroxyacetophenone

K2CO3

1,3-dibromopropane

→

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

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux 5 hours
2. 2
   أخرىThe solvent was removed
3. 3
   استخلاصThe crude product was extracted into dichloromethane (150 ml)
4. 4
   ترشيحthe insoluble inorganics were filtered off
5. 5
   تركيزThe solution was concentrated to dryness again
6. 6
   أخرىPurification
7. 7
   أخرىThe material thus obtained (2.8 g)
8. 8
   أخرىwas recrystallized twice from isopropyl ether

الإجراء التجريبي

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.

المصدر