反応 #5528

ord-c14424b657b147a5b1cf7290b793d4e0

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 under ice-
  3. 3
    温度cooling for 2 hours
  4. 4
    洗浄The reaction solution was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline
  5. 5
    乾燥dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONThen, the solvent was distilled off

実験手順

To a solution of 5-[2-(hydroxy)ethylthio]imidazo[1,2-a]pyridine (9.71 g, 50 mmoles) and triethylamine (10.5 ml, 75.3 mmoles) in methylene chloride (300 ml) was added methanesulfonyl chloride (4.26 ml, 55 mmoles) with stirring under ice-cooling and the mixture was stirred under ice-cooling for 2 hours. The reaction solution was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline and dried over anhydrous magnesium sulfate. Then, the solvent was distilled off to obtain 13.6 g of the desired product (quantitative, brown oily product).

出典

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