Reaktion #350126

Reaktionsgleichung

2-[2-bromo-N-(2,2,2-trifluoroethyl)-acetamido]-5-chloro-2'-fluorobenzophenone

hexamethylenetetramine

ammonium bromide

→

7-Chloro-1,3-dihydro-1-(2,2,2-trifluoroethyl)-5-(2'-fluorophenyl)-2H-1,4-benzodiazepin-2-one

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturReflux 1.13 g
2. 2
   Sonstige4 hours
3. 3
   Extraktionextract with dichloromethane
4. 4
   TrocknenDry the dichloromethane solution over anhydrous sodium sulfate
5. 5
   Filtrationfilter
6. 6
   Sonstigeevaporate
7. 7
   SonstigeAfter recrystallization

Vorschrift

Reflux 1.13 g. (0.0025 moles) of 2-[2-bromo-N-(2,2,2-trifluoroethyl)-acetamido]-5-chloro-2'-fluorobenzophenone, 1.4 g. (0.01 mole) of hexamethylenetetramine, and 0.98 g. (0.01 moles) of ammonium bromide together for 43/4 hours. Pour the reaction mixture into water and extract with dichloromethane. Dry the dichloromethane solution over anhydrous sodium sulfate, filter and evaporate. After recrystallization, the so-obtained 7-chloro-1,3-dihydro-1-(2,2,2-trifluoroethyl)-5-(2'fluorophenyl)-2H-1,4-benzodiazepin-2-one melts at 123°-125° C. Thin layer chromatography shows the product to be pure single spot material.

Quelle