Reacción #1884945

ord-0fbc5c7f57904aa7b5dc0e5c6e36a6ea

Ecuación de reacción

O=C(O)C(F)(F)F
Trifluoroacetic acid
NNC(=O)C(F)(F)F
trifluoroacethydrazide
O=C(NNC(=O)C(F)(F)F)C(F)(F)F
1,2-bis(trifluoroacetyl)hydrazine

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture was heated
  2. 2
    Temperaturaunder reflux for 2 h
  3. 3
    OtroA Dean and Stark trap was fitted
  4. 4
    Temperaturareflux
  5. 5
    TemperaturaReflux
  6. 6
    Otrowas continued in the absence of the Dean and Stark trap (3 h)
  7. 7
    Otro(20 h)
  8. 8
    FiltraciónThe resulting white solid was collected by filtration
  9. 9
    Otrodried in vacuum

Procedimiento

Trifluoroacetic acid (7.6 mL, 0.1 mol) was added to a stirred solution of trifluoroacethydrazide (12.8 g, 0.1 mol) in benzene (100 mL) and the mixture was heated under reflux for 2 h. A Dean and Stark trap was fitted, and reflux was continued for 3 h. Reflux was continued in the absence of the Dean and Stark trap (3 h) and then with the trap refitted (20 h). The resulting white solid was collected by filtration, dried in vacuum and identified as 1,2-bis(trifluoroacetyl)hydrazine (16.5 g, 73%). M.p. 173-175° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08343260B2uspto-grants-2013_01