Reaktion #2251

ord-dd9f79aff70f4e008da6da583aa08a55

Reaktionsgleichung

N#CN
cyanamide
Nc1cccc(C(F)(F)F)c1
3-trifluoromethyl-aniline
O=[N+]([O-])O
nitric acid
N=C(N)Nc1cccc(C(F)(F)F)c1.O=[N+]([O-])O
3-trifluoromethyl-phenylguanidine nitrate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture is heated for 20 h under RF
  2. 2
    TemperaturIt is then cooled to 0°
  3. 3
    Filtrationfiltered
  4. 4
    Waschenis washed with ethanol
  5. 5
    Sonstigedried at 60° under HV

Vorschrift

6.3 g (150 mmol) of cyanamide (50% in water) are added to a suspension of 16.1 g (100 mmol) of 3-trifluoromethyl-aniline in 35 ml of ethanol. 7.0 ml of nitric acid (65%, 0.1 mol) are then added to the brown solution and the reaction mixture is heated for 20 h under RF. It is then cooled to 0° and filtered, and the material retained on the filter is washed with ethanol and dried at 60° under HV to give 3-trifluoromethyl-phenylguanidine nitrate; 1H-NMR (dimethyl sulfoxide): 7.6 (7H,m), 9.9 (1H,br,s).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728708uspto-grants-1998_03