반응 #5185

ord-757ef081a3af49d2a9a2d7813d18eacf

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITat 25° C. for 2 hours
  2. 2
    기타the crystals which precipitated
  3. 3
    여과were collected by filtration

실험 절차

106 ml of a 4N ethyl acetate solution of hydrogen chloride were added, whilst ice-cooling, to a solution of 27.50 g of (3R)-1-t-butoxycarbonyl-3-(4-methoxybenzylthio)pyrrolidine [prepared as described in step (2) above] dissolved in 100 ml of ethyl acetate, and the mixture was stirred at 0° to 5° C. for 30 minutes and then at 25° C. for 2 hours. At the end of this time, the mixture was diluted with 200 ml of diisopropyl ether, and the crystals which precipitated were collected by filtration, to give 20.84 g of the title compound as colorless crystals, melting at 125°-126° C.

출처

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