반응 #5563

ord-4e2651d7658c4004854f8e9660ba034f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    workup.STIRRINGthe mixture was further stirred under ice-
  3. 3
    온도cooling for 10 minutes
  4. 4
    세척The reaction mixture was washed with water
  5. 5
    추출the aqueous layer was extracted with methylene chloride (30 ml×3)
  6. 6
    건조dried over anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONThen, the solvent was distilled off

실험 절차

To a solution of 5-[3-(hydroxy)propylthio]imidazo[1,2-a]pyridine (2.003 g, 9.62 mmoles) and triethylamine (2.01 ml, 14.4 mmoles) in methylene chloride (30 ml) was added methanesulfonyl chloride (0.89 ml, 12 mmoles) with stirring under ice-cooling and the mixture was further stirred under ice-cooling for 10 minutes. The reaction mixture was washed with water and the aqueous layer was extracted with methylene chloride (30 ml×3). The methylene chloride layers were combined and dried over anhydrous magnesium sulfate. Then, the solvent was distilled off to obtain crude 5-[3-(methanesulfonyloxy)propylthio]imidazo[1,2-a]pyridine as a yellow oily product.

출처

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