Reaktion #2335929

Reaktionsgleichung

water

acetoxyacetyl chloride

2-amino-6-(ethylamino)benzonitrile

pyridine

→

title compound

2-(acetoxyacetylamino)-6-(ethylamino)benzonitrile

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis cooled in an ice bath
2. 2
   Extraktionthe mixture is extracted with methylene chloride
3. 3
   TrocknenThe organic layer is dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONthe solvent is distilled off under reduced pressure
5. 5
   SonstigeThe resulting crude crystals are recrystallized from ethyl acetate-hexane

Vorschrift

To a solution of 2-amino-6-(ethylamino)benzonitrile (6.7 g) in methylene chloride (100 ml) is added pyridine (4.8 ml), and to the mixture is added dropwise acetoxyacetyl chloride (6.5 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethyl acetate-hexane to give the title compound (7.8 g) having the following physical properties.

Quelle