Réaction #992682

ord-c7156b57d90c4b4eb7ca744e436741aa

Équation de réaction

O=C(O)C(F)(F)F
Trifluoroacetic acid
N=C(N)N.O=C(O)O
Guanidine carbonate
NC(N)=[NH2+].O=C([O-])C(F)(F)F
Guanidinium TFA

Solvants

Conditions de réaction

Température
90°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.STIRRINGwith stirring as
  2. 2
    Autreto avoid bubbling over the sides of the beaker due to the evolution of carbon dioxide
  3. 3
    workup.STIRRINGThe reaction was stirred at room temperature for 2 hours
  4. 4
    AutreThe water was removed in vacuo
  5. 5
    AutreThe product was recovered as a white crystalline solid

Mode opératoire

Trifluoroacetic acid (50.0 ml, 74.0 g, 649 mmol) was added to 500 ml of distilled water in a 4-liter beaker with stirring. Guanidine carbonate (58.5 g, 324.5 mmol) was added at room temperature in portions with stirring as to avoid bubbling over the sides of the beaker due to the evolution of carbon dioxide. The reaction was stirred at room temperature for 2 hours. The water was removed in vacuo with heating to approximately 90° C. for 4 hours. The product was recovered as a white crystalline solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08012277B2uspto-grants-2011_09