Hydrazine, dihydrochloride → 4-(Trifluoromethyl)-1,2-dihydropyridazine-3,6-dione

HRID 657928Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 657928
[F:1][C:2]([F:11])([F:10])[C:3]1[C:4](=O)[O:5][C:6](=[O:8])[CH:7]=1.Cl.Cl.[NH2:14][NH2:15]>O>[F:1][C:2]([F:11])([F:10])[C:3]1[C:4](=[O:5])[NH:14][NH:15][C:6](=[O:8])[CH:7]=1

Komponenten

4

Edukt 2

HCID 17548Hydrazine, dihydrochlorideHCID 27775313-(Trifluoromethyl)furan-2,5-dione

Produkt 1

HCID 669415854-(Trifluoromethyl)-1,2-dihydropyridazine-3,6-dioneAusbeute 4,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

3-Trifluoromethylfuran-2,5-dione (5 g) was introduced in portions into an already boiling solution of hydrazine dihydrochloride (3.2 g) in water (50 ml). After stirring for 4 h, the mixture was left to stand overnight; the next day, the mixture was refluxed for a further 8 h and left to stand overnight. Then it was dried and the residue was purified by means of preparative chromatography (met. C). The clean fractions were combined, the ACN was drawn off and the residue was freeze-dried. 250 mg of the title compound were obtained. LC-MS rt: 0.23 min [M+H]+: 181.1 (met.b)

Aufarbeitung

  1. waitthe mixture was left
  2. waitto stand overnight
  3. temperaturethe next day, the mixture was refluxed for a further 8 h
  4. waitleft
  5. waitto stand overnight
  6. customThen it was dried
  7. customthe residue was purified by means of preparative chromatography (met. C)
  8. customthe residue was freeze-dried

Quellen und Nachweise

ORD-Eintrag
ord-dfe4c3c022484aa890fdf7518fc8a9b2
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08076336B2

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