Reaktion #1106607

Reaktionsgleichung

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturunder reflux for 2 h
3. 3
   SonstigeA Dean and Stark trap was fitted
4. 4
   Temperaturreflux
5. 5
   TemperaturReflux
6. 6
   Sonstigewas continued in the absence of the Dean and Stark trap (3 h)
7. 7
   Sonstige(20 h)
8. 8
   FiltrationThe resulting white solid was collected by filtration
9. 9
   Sonstigedried in vacuum

Vorschrift

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.

Quelle