反应详情

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.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 2 h
3. customA Dean and Stark trap was fitted
4. temperaturereflux
5. temperatureReflux
6. customwas continued in the absence of the Dean and Stark trap (3 h)
7. custom(20 h)
8. filtrationThe resulting white solid was collected by filtration
9. customdried in vacuum