반응 #3600

ord-0324d1ccc345444c9eb2d3d9fc2f1123

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The mixture is washed with water, and 1M NaHCO3 and dried(Na2 SO4)
  2. 2
    기타The solvent is removed in vacuo
  3. 3
    기타to give a solid which
  4. 4
    기타is recrystallized from dichloromethane-hexane
  5. 5
    기타to give crystals, 185°-187° C.

실험 절차

A mixture of 1 mmol of 3-chloro-10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2 mmol of triethylamine, and 1.1 mmol of 2-methylbenzoylchloride in 8 ml of dichloromethane is stirred at room temperature overnight. The mixture is washed with water, and 1M NaHCO3 and dried(Na2 SO4). The solvent is removed in vacuo to give a solid which is recrystallized from dichloromethane-hexane to give crystals, 185°-187° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733905uspto-grants-1998_03