反応 #5529

ord-824f8a15b5d240dc96f33facfa1f2b99

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度at reflux for 3 hours
  2. 2
    洗浄The reaction solution was washed with an aqueous 3N-sodium hydroxide solution
  3. 3
    乾燥dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONAfter the solvent was distilled off
  5. 5
    その他the residue was purified by column chromatography (eluent: methanol/chloroform=1:10)

実験手順

A solution of 5-[2-(methylsulfonyloxy)ethylthio]imidazo[1,2-a]pyridine (2.18 g, 8 mmoles), triethylamine (2.24 ml, 16 mmoles) and a 40% methylamine-methanol solution (20 ml) in chloroform (20 ml) was heated at reflux for 3 hours. The reaction solution was washed with an aqueous 3N-sodium hydroxide solution and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: methanol/chloroform=1:10) to obtain 781 mg of the desired product (47.1%, light brown oily product).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05244908uspto-grants-1993_09