Reaktion #570395

ord-46cec997d2c14e218dcae9cba917f059

Lösungsmittel

Reaktionsbedingungen

Temperatur
10°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturWhen the mixture was heated
  2. 2
    Sonstigea homogeneous solution was first obtained
  3. 3
    Sonstigeto form in the mixture
  4. 4
    TemperaturAfter 30 minutes at reflux
  5. 5
    Temperaturto cool
  6. 6
    workup.STIRRINGwith stirring
  7. 7
    Sonstigethe solid was separated by filtration
  8. 8
    Sonstigedried in a vacuum oven overnight

Vorschrift

To a solution of 210 g of hydrazine dihydrochloride in 2 liters of water there was added, in one portion, 224 g of citraconic anhydride. When the mixture was heated to boiling with stirring, a homogeneous solution was first obtained and then a white precipitate started to form in the mixture. After 30 minutes at reflux, the mixture was allowed to cool with stirring. It was then cooled to 10° C. and the solid was separated by filtration and dried in a vacuum oven overnight to give citraconic hydrazide melting at about 281-283.5° C. with decomposition.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04578464uspto-grants-1986_03