Reaktion #218518

Reaktionsgleichung

2-(4,5-difluoro-2-nitro-phenylamino)-5-trifluoromethyl-benzonitrile

tin (II) chloride

→

title compound

Ausbeute 64.0%

7,8-Difluoro-2-trifluoromethyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride

Ausbeute 64.0%

Lösungsmittel

ethanol

hydrochloric acid

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturHeat the resulting mixture
2. 2
   Temperaturto reflux for 18 hours
3. 3
   TemperaturCool
4. 4
   Sonstigethe reaction to room temperature
5. 5
   FiltrationCollect by filtration the precipitated product from the solution
6. 6
   WaschenWash solid with 5.0 N hydrochloric acid

Vorschrift

Heat a solution of 2-(4,5-difluoro-2-nitro-phenylamino)-5-trifluoromethyl-benzonitrile (0.995 g, 2.90 mmol) in ethanol (15 ml) to 60° C. Add to this a solution of tin (II) chloride (1.65 g, 8.70 mmol) in 5.0 N hydrochloric acid (15 ml). Heat the resulting mixture to reflux for 18 hours. Cool the reaction to room temperature, add 30 ml of 5.0 N hydrochloric acid and place the mixture in a freezer for 16 hours. Collect by filtration the precipitated product from the solution. Wash solid with 5.0 N hydrochloric acid to obtain 0.648 g of the title compound (1.85 mmol, 64% yield) as a yellow amorphous solid: Mass Spectrum (m/e): 314(M+1).

Quelle