반응 #1546711

ord-42eb715f38324593ae4c52f488d2c935

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heating
  2. 2
    온도under reflux for 3 hours
  3. 3
    여과The reaction mixture is filtered through diatomaceous earth
  4. 4
    농축The filtrate is concentrated in vacuo to a residue which
  5. 5
    workup.DISSOLUTIONis dissolved in methylene chloride
  6. 6
    농축The filtrate is concentrated in vacuo

실험 절차

To a solution of 5 mmol of 6,7-dihydro-5-(4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 25 ml of ethyl alcohol is added 0.3 g of 10% Pd/C and 15 mmol of hydrazine followed by stirring and heating under reflux for 3 hours. The reaction mixture is filtered through diatomaceous earth. The filtrate is concentrated in vacuo to a residue which is dissolved in methylene chloride and passed through a pad of hydrous magnesium silicate. The filtrate is concentrated in vacuo to give the desired product which is purified by flash chromatography on silica gel to give the desired product as a solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05854237uspto-grants-1998_12