Hydrazine, dihydrochloride → 4-(Trifluoromethyl)-1,2-dihydropyridazine-3,6-dione

HRID 1524521ノート

反応式

HRID 1524521 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[C:4](=O)[O:5][C:6](=[O:8])[CH:7]=1.Cl.Cl.[NH2:14][NH2:15]>O>[F:1][C:2]([F:11])([F:10])[C:3]1[C:4](=[O:5])[NH:14][NH:15][C:6](=[O:8])[CH:7]=1

参加物

4

反応物 2

HCID 17548Hydrazine, dihydrochlorideHCID 27775313-(Trifluoromethyl)furan-2,5-dione

生成物 1

HCID 669415854-(Trifluoromethyl)-1,2-dihydropyridazine-3,6-dione収率 4.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-Trifluoromethylfuran-2,5-dione (5 g) was introduced in portions into an already boiling solution of hydrazine dihydrochloride (3.2 g) in water (50 ml). After stirring for 4 h, the mixture was left to stand overnight; the next day, the mixture was refluxed for a further 8 h and left to stand overnight. Then it was dried and the residue was purified by means of preparative chromatography (met. C). The clean fractions were combined, the ACN was drawn off and the residue was freeze-dried. 250 mg of the title compound were obtained. LC-MS rt: 0.23 min

後処理

  1. waitthe mixture was left
  2. waitto stand overnight
  3. temperaturethe next day, the mixture was refluxed for a further 8 h
  4. waitleft
  5. waitto stand overnight
  6. customThen it was dried
  7. customthe residue was purified by means of preparative chromatography (met. C)
  8. customthe residue was freeze-dried

出典と根拠

ORDレコード
ord-3bd6395cb78b42e4a5f842afd4db3e34
出典データセット
uspto-grants-2015_07
特許番号
US09079906B2

反応ノート

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