Reaktion #992682

ord-c7156b57d90c4b4eb7ca744e436741aa

Reaktionsgleichung

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

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGwith stirring as
  2. 2
    Sonstigeto 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
    SonstigeThe water was removed in vacuo
  5. 5
    SonstigeThe product was recovered as a white crystalline solid

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08012277B2uspto-grants-2011_09