反应 #92930

反应方程式

1-bromo-2-(3-ethoxyphenyl)-2-oxoethane

1-methylimidazole

→

1-methyl-3-[2-(3-ethoxyphenyl)-2-oxoethyl]-1H-imidazolium bromide

收率 7.0%

溶剂

methanol

acetonitrile

反应条件

后处理

1. 1
   其他the volatiles were evaporated under reduced pressure to a volume of approximately 15 ml
2. 2
   workup.ADDITIONThis solution was diluted with ethyl acetate
3. 3
   过滤the precipitated brown solid was collected by filtration
4. 4
   洗涤The collected solid was washed with ethyl acetate
5. 5
   workup.DISSOLUTIONdissolved in hot acetonitrile
6. 6
   其他The mixture was purified with charcoal
7. 7
   温度upon cooling the solid
8. 8
   其他was collected
9. 9
   其他The solid was recrystallized from acetonitrile/diethyl ether
10. 10
    其他to provide two crops which
11. 11
    其他recrystallized three times from isopropyl alcohol

实验过程

A solution of 2.9 g (0.012 mol) of 1-bromo-2-(3-ethoxyphenyl)-2-oxoethane in 20 ml of acetonitrile was combined with 1.03 g (0.013 mol) of 1-methylimidazole and the resulting mixture was stirred at room temperature for approximately 18 hours. The mixture was diluted with methanol and the volatiles were evaporated under reduced pressure to a volume of approximately 15 ml. This solution was diluted with ethyl acetate and the precipitated brown solid was collected by filtration. The collected solid was washed with ethyl acetate and dissolved in hot acetonitrile. The mixture was purified with charcoal and upon cooling the solid was collected. The solid was recrystallized from acetonitrile/diethyl ether to provide two crops which were combined and recrystallized three times from isopropyl alcohol to afford 0.27 g of 1-methyl-3-[2-(3-ethoxyphenyl)-2-oxoethyl]-1H-imidazolium bromide as pale yellow flakes. (7% yield) mp=137°-138° C.

来源