反应 #1106607

ord-dc8fa5cbd166445cb6dbc2f280a80cfe

反应方程式

O=C(O)C(F)(F)F
Trifluoroacetic acid
NNC(=O)C(F)(F)F
trifluoroacethydrazide
O=C(NNC(=O)C(F)(F)F)C(F)(F)F
1,2-bis(trifluoroacetyl)hydrazine

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08715395B2uspto-grants-2014_05