Reaktion #745110

Reaktionsgleichung

3-Trifluoromethylfuran-2,5-dione

hydrazine dihydrochloride

→

title compound

Ausbeute 4.6%

4-Trifluoromethyl-1,2-dihydropyridazin-3,6-dione

Ausbeute 4.6%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITthe mixture was left
2. 2
   workup.WAITto stand overnight
3. 3
   Temperaturthe next day, the mixture was refluxed for a further 8 h
4. 4
   workup.WAITleft
5. 5
   workup.WAITto stand overnight
6. 6
   SonstigeThen it was dried
7. 7
   Sonstigethe residue was purified by means of preparative chromatography (met. C)
8. 8
   Sonstigethe residue was freeze-dried

Vorschrift

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)

Quelle