Ammonia → 3,5-Dichloro-1,4-dihydropyridazin-4-imine

HRID 568308ノート

反応式

HRID 568308 の反応式
[NH3:1].[Cl:2][C:3]1[N:4]=[N:5][CH:6]=[C:7]([Cl:10])[C:8]=1Cl>C(O)C>[NH2:1][C:8]1[C:7]([Cl:10])=[CH:6][N:5]=[N:4][C:3]=1[Cl:2]

参加物

4

反応物 2

HCID 222AmmoniaHCID 701113,4,5-Trichloropyridazine

生成物 1

HCID 64032013,5-Dichloro-1,4-dihydropyridazin-4-imine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dry ethanol is saturated with ammonia gas and placed in a sealed tube with 8.0 grams of 3,4,5-trichloropyridazine. The reaction mixture is heated at 120°-130° C. for five hours. The tube is opened and the reaction mixture concentrated under reduced pressure. The residue is dissolved in 20 ml of chloroform and the solution heated under reflux for 20 minutes. The solution is allowed to cool to ambient temperature for several hours in place. A solid precipitate is collected by filtration and repeatedly recrystallized from water to yield 2.8 grams of 4-amino-3,5-dichloropyridazine; m.p. 176°-178° C. The filtrate is concentrated under reduced pressure and the residue recrystallized from water to yield 2.0 grams of 4-amino-5,6-dichloropyridazine; m.p. 150°-151° C.

後処理

  1. temperatureThe reaction mixture is heated at 120°-130° C. for five hours
  2. concentrationthe reaction mixture concentrated under reduced pressure
  3. dissolutionThe residue is dissolved in 20 ml of chloroform
  4. temperaturethe solution heated
  5. temperatureunder reflux for 20 minutes
  6. filtrationA solid precipitate is collected by filtration
  7. customrepeatedly recrystallized from water

出典と根拠

ORDレコード
ord-91bb49642bac4ae988c8ba2ee8d5982e
出典データセット
uspto-grants-1988_03
特許番号
US04728355

反応ノート

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