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

HRID 657928ノート

反応式

HRID 657928 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 [M+H]+: 181.1 (met.b)

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-dfe4c3c022484aa890fdf7518fc8a9b2
出典データセット
uspto-grants-2011_12
特許番号
US08076336B2

反応ノート

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