反応 #43446

ord-d45f37f166944474839658fa69d9d642

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated
  2. 2
    温度to reflux
  3. 3
    温度The mixture was heated
  4. 4
    温度at reflux for 4 hours
  5. 5
    ろ過The precipitates were collected by filtration
  6. 6
    洗浄washed with water and acetone
  7. 7
    その他dried as a combined batch in vacuo

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07732460B2uspto-grants-2010_06