Reaktion #43446

ord-d45f37f166944474839658fa69d9d642

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturto reflux
  3. 3
    TemperaturThe mixture was heated
  4. 4
    Temperaturat reflux for 4 hours
  5. 5
    FiltrationThe precipitates were collected by filtration
  6. 6
    Waschenwashed with water and acetone
  7. 7
    Sonstigedried as a combined batch in vacuo

Vorschrift

Hydrazine sulphate salt (51 g) was suspended in water (250 ml), heated to reflux and bromomaleic anhydride (90.38 g) was added dropwise. The mixture was heated at reflux for 4 hours then cooled to room temperature. The reaction was repeated with 29 g hydrazine sulphate, 53 g bromomaleic anhydride and 130 ml water. The precipitates were collected by filtration, washed with water and acetone and dried as a combined batch in vacuo to afford 4-bromo-1,2-dihydro-3,6-pyridazinedione as a white solid (113 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732460B2uspto-grants-2010_06