Реакция #1884945
ord-0fbc5c7f57904aa7b5dc0e5c6e36a6ea
Уравнение реакции
Trifluoroacetic acid
trifluoroacethydrazide
→
1,2-bis(trifluoroacetyl)hydrazine
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураthe mixture was heated
- 2Температураunder reflux for 2 h
- 3ДругоеA Dean and Stark trap was fitted
- 4Температураreflux
- 5ТемператураReflux
- 6Другоеwas continued in the absence of the Dean and Stark trap (3 h)
- 7Другое(20 h)
- 8ФильтрацияThe resulting white solid was collected by filtration
- 9Другоеdried 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.