Реакция #1106607

Уравнение реакции

Trifluoroacetic acid

trifluoroacethydrazide

→

1,2-bis(trifluoroacetyl)hydrazine

Растворители

benzene

Условия реакции

Обработка

1. 1
   Температураthe mixture was heated
2. 2
   Температураunder reflux for 2 h
3. 3
   ДругоеA Dean and Stark trap was fitted
4. 4
   Температураreflux
5. 5
   ТемператураReflux
6. 6
   Другоеwas continued in the absence of the Dean and Stark trap (3 h)
7. 7
   Другое(20 h)
8. 8
   ФильтрацияThe resulting white solid was collected by filtration
9. 9
   Другоеdried in vacuum

Методика

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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