Reaction #1106607

Reaction equation

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

Solvents

benzene

Conditions

Workup

1. 1
   Temperaturethe mixture was heated
2. 2
   Temperatureunder reflux for 2 h
3. 3
   OtherA Dean and Stark trap was fitted
4. 4
   Temperaturereflux
5. 5
   TemperatureReflux
6. 6
   Otherwas continued in the absence of the Dean and Stark trap (3 h)
7. 7
   Other(20 h)
8. 8
   FiltrationThe resulting white solid was collected by filtration
9. 9
   Otherdried in vacuum

Procedure

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.

Source