반응 #43446

ord-d45f37f166944474839658fa69d9d642

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도to reflux
  3. 3
    온도The mixture was heated
  4. 4
    온도at reflux for 4 hours
  5. 5
    여과The precipitates were collected by filtration
  6. 6
    세척washed with water and acetone
  7. 7
    기타dried as a combined batch in vacuo

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732460B2uspto-grants-2010_06