반응 #5554

ord-60c2ecf6995d45a5aa4ac142f572040a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05244908uspto-grants-1993_09