Reaktion #5675

Reaktionsgleichung

5-dimethylamino-2,3,4,5-tetrahydro-1H-benzazepine

potassium carbonate

p-nitrobenzoyl chloride

→

5-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine

Ausbeute 97.1%

Lösungsmittel

water

acetone

water

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle