反应 #1884945
ord-0fbc5c7f57904aa7b5dc0e5c6e36a6ea
反应方程式
Trifluoroacetic acid
trifluoroacethydrazide
→
1,2-bis(trifluoroacetyl)hydrazine
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度the mixture was heated
- 2温度under reflux for 2 h
- 3其他A Dean and Stark trap was fitted
- 4温度reflux
- 5温度Reflux
- 6其他was continued in the absence of the Dean and Stark trap (3 h)
- 7其他(20 h)
- 8过滤The resulting white solid was collected by filtration
- 9其他dried in vacuum
实验过程
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.