Reaction #992682

ord-c7156b57d90c4b4eb7ca744e436741aa

Reaction equation

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

Solvents

Conditions

Temperature
90°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

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

Procedure

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.v1Patent: US08012277B2uspto-grants-2011_09