Reaktion #304888

ord-6a40094369a44c53991baf5d098a651f

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThen the mixture was heated
  2. 2
    Temperaturto reflux for 3 h
  3. 3
    SonstigeSubsequently, the precipitate formed
  4. 4
    Filtrationwas filtered off with suction
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigedried
  7. 7
    Filtrationfiltered off with suction
  8. 8
    Sonstigedried

Vorschrift

Hydrazine dihydrochloride (83.6 g) was dissolved in water (20 ml) and heated to 100° C., and 3,4-dimethylfuran-2,5-dione (100.4 g) was introduced while stirring. Then the mixture was heated to reflux for 3 h. Subsequently, the precipitate formed was filtered off with suction, washed with water and dried. The residue was suspended in EA (2 l), filtered off with suction and dried. 69.7 g of the title compound were obtained. LC-MS rt: 0.19 min[M+H]+: 141.1 (met. b)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08198272B2uspto-grants-2012_06