反応 #4631

ord-c809392bdfff4c2c992ddff80aae92cb

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated at a bath temperature of 140°
  2. 2
    workup.WAITboiling is continued for a further hour
  3. 3
    workup.WAITThe solution is then left
  4. 4
    workup.DISTILLATIONis distilled off in vacuo
  5. 5
    workup.DISTILLATIONA sample of the oil remaining was distilled in a bulb tube
  6. 6
    その他Boiling point, bath temperature 120°/0.06 torr

実験手順

38.5 g of 2-benzyloxybenzylamine hydrochloride are suspended in 400 ml of distilled toluene and heated at a bath temperature of 140°. Whilst stirring, phosgene is introduced and after about 50 minutes the solution becomes clear. After a further 10 minutes, the addition of phosgene is interrupted and boiling is continued for a further hour. The solution is then left to cool a little and the toluene is distilled off in vacuo. A sample of the oil remaining was distilled in a bulb tube: Boiling point, bath temperature 120°/0.06 torr.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727067uspto-grants-1988_02