Hydrazine hydrate (1:1) → HCID 178434193, Verbindung

HRID 1700640Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1700640
[Cl:1][C:2]1[S:3][C:4]([Cl:18])=[CH:5][C:6]=1[CH:7]1[CH2:12][C:11](=O)[C:10](=[C:14](O)[CH3:15])[C:9](=[O:17])[CH2:8]1.O.[NH2:20][NH2:21]>C(O)C>[Cl:1][C:2]1[S:3][C:4]([Cl:18])=[CH:5][C:6]=1[CH:7]1[CH2:12][C:11]2[NH:21][N:20]=[C:14]([CH3:15])[C:10]=2[C:9](=[O:17])[CH2:8]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 178467259HCID 178467259, Verbindung

Produkt 1

HCID 178434193HCID 178434193, VerbindungAusbeute 87,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 5-(2,5-dichlorothiophen-3-yl)-2-(1-hydroxyethylidene)cyclohexane-1,3-dione (2.48 g) and hydrazine hydrate (0.508 g) in ethanol (10 ml) was refluxed for 2 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and concentrated under reduced pressure. The residue was washed with diisopropylether to give 6-(2,5-dichlorothiophen-3-yl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (2.15 g) as pale yellow crystals.

Aufarbeitung

  1. customUnder reduced pressure, the solvent was evaporated
  2. additionto the residue was added water
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe organic layer was washed with water
  5. concentrationconcentrated under reduced pressure
  6. washThe residue was washed with diisopropylether

Quellen und Nachweise

ORD-Eintrag
ord-df408351dde541fbad1a26fda9ba44ec
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06350749B1

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