Hydrazine → HCID 178434976, Verbindung

HRID 2120859Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2120859
[CH3:1][C:2]1[O:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3]=1[C:13](=O)[CH2:14][C:15]#[N:16].[NH2:18][NH2:19]>C(O)C>[CH3:1][C:2]1[O:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3]=1[C:13]1[CH:14]=[C:15]([NH2:16])[NH:18][N:19]=1

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 234356403-(5-Methyl-3-phenyl-isoxazol-4-yl)-3-oxo-propionitrile

Produkt 1

HCID 178434976HCID 178434976, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

3-(5-Methyl-3-phenyl-isoxazol-4-yl)-3-oxo-propionitrile (0.391 g, 1.73 mmol) in Ethanol (3 mL) was treated with hydrazine (0.168 mL, 3.46 mmol) and heated to reflux. Evaporation in vacuum gave 5-(5-Methyl-3-phenyl-isoxazol-4-yl)-2H-pyrazol-3-ylamine used without purification. To the resulting amine (0.039 g, 0.16 mmol) in dioxane was added triethyl amine followed by benzyl chloride (0.019 mL, 0.16 mmol). The reaction was stirred at 10° C. for 1 hr and 2 hr at ambient temperature. The solution was diluted with water extracted with ethyl acetate, washed with saturated NaHCO3, Brine, dried over MgSO4 and concentrated in vacuum. HPLC purification afforded 1.4 mg of title compound.

Aufarbeitung

  1. temperatureheated to reflux
  2. customEvaporation in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-1b055e63efa34962a7957052dd9a5972
Quelldatensatz
uspto-grants-2004_02
Patentnummer
US06693108B2

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