تفاعل #92930

معادلة التفاعل

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

1-methylimidazole

→

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

المردود 7.0%

المذيبات

methanol

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   أخرىthe 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
   ترشيحthe precipitated brown solid was collected by filtration
4. 4
   غسيلThe collected solid was washed with ethyl acetate
5. 5
   workup.DISSOLUTIONdissolved in hot acetonitrile
6. 6
   أخرىThe mixture was purified with charcoal
7. 7
   درجة الحرارةupon cooling the solid
8. 8
   أخرىwas collected
9. 9
   أخرىThe solid was recrystallized from acetonitrile/diethyl ether
10. 10
    أخرىto provide two crops which
11. 11
    أخرىrecrystallized three times from isopropyl alcohol

الإجراء التجريبي

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.

المصدر