반응 #5211

ord-c4ffa53c53ad4c46a62aa45858110c76

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타At the end of this time, the crystals which precipitated
  2. 2
    여과were collected by filtration
  3. 3
    세척washed with tetrahydrofuran
  4. 4
    건조dried over anhydrous magnesium sulfate
  5. 5
    기타the solvent was removed by distillation under reduced pressure

실험 절차

1.06 ml of triethylamine and subsequently 584 μl of methanesulfonyl chloride were added, whilst ice-cooling, to a solution of 2.13 g of (2S, 4S)-1-(2-hydroxyethyl)-4-(4-methoxybenzylthio)-2-methylcarbamoylpyrrolidine dissolved in 45 ml of dry tetrahydrofuran, and the mixture was stirred at 0° to 5° C. for 30 minutes. At the end of this time, the crystals which precipitated were collected by filtration and washed with tetrahydrofuran. The filtrate and washings were combined and dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure, to afford 2.50 g of the title compound as an oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05242914uspto-grants-1993_09