反応 #5554

ord-60c2ecf6995d45a5aa4ac142f572040a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooling
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
  3. 3
    洗浄The reaction mixture was washed in turn with an aqueous sodium bicarbonate solution and water
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONAfter the solvent was distilled off
  6. 6
    その他the residue was purified by column chromatography (eluent: ethyl acetate)

実験手順

To a solution of 5-[4-(amino)butylthio]imidazo[1,2-a]pyridine (300 mg, 1.36 mmoles) and triethylamine (0.29 ml, 2.08 mmoles) in methylene chloride (15 ml) was added 1-naphthalenesulfonyl chloride (307 mg, 1.35 mmoles) under ice-cooling with stirring and the mixture was stirred at room temperature for 1 hour. The reaction mixture was washed in turn with an aqueous sodium bicarbonate solution and water and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate) to obtain 296 mg of the desired product (53.0%, colorless solid).

出典

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