Trifluoroacetic acid → 2,2,2-Trifluoro-N'-(trifluoroacetyl)acetohydrazide

HRID 1797763Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1797763
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=O.[F:8][C:9]([F:15])([F:14])[C:10]([NH:12][NH2:13])=[O:11]>C1C=CC=CC=1>[F:8][C:9]([F:15])([F:14])[C:10]([NH:12][NH:13][C:3](=[O:5])[C:2]([F:7])([F:6])[F:1])=[O:11]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 229753Trifluoroacetohydrazide

Produkt 1

HCID 2297542,2,2-Trifluoro-N'-(trifluoroacetyl)acetohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 h
  3. customA Dean and Stark trap was fitted
  4. temperaturereflux
  5. temperatureReflux
  6. customwas continued in the absence of the Dean and Stark trap (3 h)
  7. custom(20 h)
  8. filtrationThe resulting white solid was collected by filtration
  9. customdried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-0fbc5c7f57904aa7b5dc0e5c6e36a6ea
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08343260B2

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