반응 #3631

ord-e3bdc34f4e1540a0adc207a4fc060fb9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heating
  2. 2
    온도under reflux for 3 hours
  3. 3
    기타The room temperature reaction mixture
  4. 4
    여과is filtered through diatomaceous earth
  5. 5
    농축the filtrate concentrated in vacuo
  6. 6
    workup.DISSOLUTIONThe residue is dissolved in methylene chloride
  7. 7
    농축The filtrate is concentrated in vacuo

실험 절차

To a solution of 1 mmol of 9,10-dihydro-10-(4-nitrobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine in 20 ml of ethyl alcohol is added 0.2 g of 10% Pd/C and 2.5 mmol of hydrazine followed by stirring and heating under reflux for 3 hours. The room temperature reaction mixture is filtered through diatomaceous earth and the filtrate concentrated in vacuo. The residue is dissolved in methylene chloride and passed through a thin 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: US05733905uspto-grants-1998_03