Réaction #1106607

Équation de réaction

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

Solvants

benzene

Conditions de réaction

Traitement

1. 1
   Températurethe mixture was heated
2. 2
   Températureunder reflux for 2 h
3. 3
   AutreA Dean and Stark trap was fitted
4. 4
   Températurereflux
5. 5
   TempératureReflux
6. 6
   Autrewas continued in the absence of the Dean and Stark trap (3 h)
7. 7
   Autre(20 h)
8. 8
   FiltrationThe resulting white solid was collected by filtration
9. 9
   Autredried in vacuum

Mode opératoire

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