반응 #1884945

반응 방정식

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

용매

benzene

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux for 2 h
3. 3
   기타A Dean and Stark trap was fitted
4. 4
   온도reflux
5. 5
   온도Reflux
6. 6
   기타was continued in the absence of the Dean and Stark trap (3 h)
7. 7
   기타(20 h)
8. 8
   여과The resulting white solid was collected by filtration
9. 9
   기타dried in vacuum

실험 절차

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.

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