Réaction #5675

ord-e5cdc5322a3f49ad962f9c48c672d656

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurecooling
  2. 2
    workup.STIRRINGthe mixture is stirred at room temperature overnight
  3. 3
    Filtrationthe precipitated crystals are collected by filtration
  4. 4
    Autredried

Mode opératoire

To a solution of 5-dimethylamino-2,3,4,5-tetrahydro-1H-benzazepine (50 g) in a mixture of acetone (400 ml) and water (200 ml) is added potassium carbonate (38.8 g), and thereto is added p-nitrobenzoyl chloride (40 g) with stirring under ice-cooling, and the mixture is stirred at room temperature overnight. To the reaction mixture is added an appropriate amount of water, and the precipitated crystals are collected by filtration and dried to give 5-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (71 g) as pale yellow powder, mp. 139°-142° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05244898uspto-grants-1993_09