Реакция #1884945

ord-0fbc5c7f57904aa7b5dc0e5c6e36a6ea

Уравнение реакции

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

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08343260B2uspto-grants-2013_01