反応 #92934

ord-adb1937ba43f4ec58485f7a79e1b4121

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The precipitated solid was collected by filtration
  2. 2
    洗浄washed with diethyl ether
  3. 3
    workup.DISSOLUTIONdissolved in methanol
  4. 4
    workup.ADDITIONThis solution was diluted with diethyl ether
  5. 5
    ろ過the resulting white solid was collected by filtration
  6. 6
    その他This solid was recrystallized from methanol/diethyl ether

実験手順

A solution of 8 ml (0.047 mol) of 90% pure 1-phenyl-1-oxo-2-bromopropane and 4.25 g (0.052 mol) of 1-methylimidazole in 100 ml of diethyl ether was stirred at room temperature for approximately 24 hours. The precipitated solid was collected by filtration, washed with diethyl ether and dissolved in methanol. This solution was diluted with diethyl ether and the resulting white solid was collected by filtration. This solid was recrystallized from methanol/diethyl ether to afford 7.65 g of 1-methyl-3-(1-methyl-2-phenyl-2-oxoethyl)-1H-imidazolium bromide as white crystals. (55% yield) mp=167°-170° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04609670uspto-grants-1986_09