Hydrazine hydrate (1:1) → HCID 178497263, Verbindung

HRID 1178144

Reaktionsgleichung

Reaktionsgleichung von HRID 1178144
[NH2:1][NH2:2].O.[CH2:4]([O:6][C:7](=[O:19])[C:8](=O)[CH2:9][C:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)C>CO>[CH3:4][O:6][C:7]([C:8]1[CH:9]=[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[NH:2][N:1]=1)=[O:19]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 2265032,4-Dioxo-4-phenyl-butyric acid ethyl ester

Produkt 1

HCID 178497263HCID 178497263, VerbindungAusbeute 77,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

NH2—NH2—H2O (1.0 g, 20 mmol) was added to a solution of 2,4-dioxo-4-phenyl-butyric acid ethyl ester (1.94 g, 8.81 mmol) in methanol (17 mL). The resulting reaction mixture was heated to reflux for two and half hours. The methanol was evaporated and the resulting solid was heated with 2.5% ethyl acetate in hexane to afford 5-phenyl-1H-pyrazole-3-carboxylic acid methyl ester as a solid in 77.3% yield. LC-MS purity: 93.345%.

Aufarbeitung

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux for two and half hours
  4. customThe methanol was evaporated
  5. temperaturethe resulting solid was heated with 2.5% ethyl acetate in hexane

Quellen und Nachweise

ORD-Eintrag
ord-249678e1f54b485bb3589580bf01fba9
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07842696B2

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