반응 #5530

ord-689b4b2ef67943d4b073104bea7fe4b7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONAfter the solvent was distilled off
  2. 2
    workup.ADDITIONethanol (15 ml) and ether (30 ml) were added to the residue
  3. 3
    기타Then, the crystals precipitated
  4. 4
    여과were filtered off
  5. 5
    세척washed in turn with ether

실험 절차

To a suspension of 5-[3-(tert-butoxycarbonylamino)propylamino]imidazo[1,2-a]pyridine (1.742 g, 6 mmoles) in methylene chloride (40 ml) was added hydrogen chloride-methanol (6 ml) and the mixture was stirred at room temperature for 20 hours. After the solvent was distilled off, ethanol (15 ml) and ether (30 ml) were added to the residue. Then, the crystals precipitated were filtered off and washed in turn with ether and a small amount of ethanol to obtain 1.311 g of the desired product (83.0%, pale yellow crystals).

출처

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