反応 #5530

ord-689b4b2ef67943d4b073104bea7fe4b7

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  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
    その他Then, the crystals precipitated
  4. 4
    ろ過were filtered off
  5. 5
    洗浄washed in turn with ether

実験手順

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).

出典

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