Reaktion #350124

Reaktionsgleichung

isopropyl alcohol

2-(2-bromoacetamido)-5-chlorobenzophenone

hexamethylenetetramine

ammonium bromide

→

7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturReflux 1.76 g
2. 2
   Extraktionextract with benzene
3. 3
   TrocknenDry the benzene solution over anhydrous sodium sulfate
4. 4
   FiltrationFilter
5. 5
   Sonstigeevaporate to dryness
6. 6
   SonstigeAfter recrystallization

Vorschrift

Reflux 1.76 g. (0.005 moles) of 2-(2-bromoacetamido)-5-chlorobenzophenone, 2.80 g. (0.02 moles) of hexamethylenetetramine and 1.96 g. (0.020 moles) of ammonium bromide in 14 ml. of 85% (v/v) aqueous isopropyl alcohol for 2 hours. Pour the reaction mixture into water and extract with benzene. Dry the benzene solution over anhydrous sodium sulfate. Filter and evaporate to dryness. After recrystallization, 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one is obtained. In thin layer chromatography the product shows a single spot (silica gel GF plates, benzene-ethyl acetate-acetic acid=18:3:1), m.p. 213°-215° C.

Quelle