반응 #92930

반응 방정식

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

1-methylimidazole

→

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

수율 7.0%

용매

methanol

acetonitrile

반응 조건

후처리

1. 1
   기타the 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
   여과the precipitated brown solid was collected by filtration
4. 4
   세척The collected solid was washed with ethyl acetate
5. 5
   workup.DISSOLUTIONdissolved in hot acetonitrile
6. 6
   기타The mixture was purified with charcoal
7. 7
   온도upon cooling the solid
8. 8
   기타was collected
9. 9
   기타The solid was recrystallized from acetonitrile/diethyl ether
10. 10
    기타to provide two crops which
11. 11
    기타recrystallized three times from isopropyl alcohol

실험 절차

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.

출처