反応 #1106607

反応方程式

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

溶媒

benzene

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度under reflux for 2 h
3. 3
   その他A Dean and Stark trap was fitted
4. 4
   温度reflux
5. 5
   温度Reflux
6. 6
   その他was continued in the absence of the Dean and Stark trap (3 h)
7. 7
   その他(20 h)
8. 8
   ろ過The resulting white solid was collected by filtration
9. 9
   その他dried in vacuum

実験手順

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.

出典