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

HRID 657928노트

반응식

HRID 657928 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-dfe4c3c022484aa890fdf7518fc8a9b2
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076336B2

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