反応 #83430

ord-03a6b4230016431fa7c2b186b3613d08

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The mixture is washed with water, and 1M NaHCO3 and dried(Na2SO4)
  2. 2
    その他The solvent is removed in vacuo
  3. 3
    その他to give a solid which
  4. 4
    その他is recrystallized from dichloromethane-hexane
  5. 5
    その他to give crystals, 185°-187° C.

実験手順

A mixture of 1 mmol of 3-chloro-10,11-di-hydro-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(Na2SO4). The solvent is removed in vacuo to give a solid which is recrystallized from dichloromethane-hexane to give crystals, 185°-187° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05624923uspto-grants-1997_04