反応 #215030

ord-6707b344290248e1bd3aceb6b5d5d863

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度to reflux for 5 minutes
  3. 3
    その他The cooled reaction mixture
  4. 4
    workup.ADDITIONwas poured on ice
  5. 5
    抽出extracted with methylene chloride
  6. 6
    その他The extracts were dried
  7. 7
    その他evaporated
  8. 8
    その他the residue was crystallized from ether/2-propanol
  9. 9
    その他to yield yellow crystals

実験手順

A mixture of 4.2 g (0.01 mole) of 7-chloro-5-(2-fluorophenyl)-2,3-dihydro-N-hydroxy-α-(4-morpholinyl)-1H-1,4-benzodiazepine-2-methanimine 4-oxide, 50 ml of glacial acetic acid and 4 ml of acetaldehyde was heated to reflux for 5 minutes. The cooled reaction mixture was poured on ice, made alkaline with ammonia and extracted with methylene chloride. The extracts were dried and evaporated and the residue was crystallized from ether/2-propanol to yield yellow crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04257946uspto-grants-1981_03