Hydrazine → HCID 178507285, Verbindung

HRID 1943905Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1943905
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=O)[CH2:8][C:9]#[N:10].[NH2:12][NH2:13]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[CH:8]=[C:9]([NH2:10])[NH:13][N:12]=1

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 115718233-Oxo-3-(pyridin-2-yl)propanenitrile

Produkt 1

HCID 178507285HCID 178507285, VerbindungAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

3-(2-Pyridyl)-3-oxopropanenitrile (3.0 g, 0.37 mol) was dissolved in ethanol (22 mL) and treated with hydrazine (1.9 mL, 0.062 mol) at reflux for 24 hours. The reaction mixture was concentrated, diluted with brine and extracted into ethyl acetate (2×50 mL). The combined organic layers were dried (MgSO4), concentrated and purified by silica gel chromatography eluting with 2-20% methanol in methylene chloride to afford 3-(pyridin-2-yl)-1H-pyrazol-5-amine (3.0 g, 91% yield).

Aufarbeitung

  1. temperatureat reflux for 24 hours
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with brine
  4. extractionextracted into ethyl acetate (2×50 mL)
  5. dry with materialThe combined organic layers were dried (MgSO4)
  6. concentrationconcentrated
  7. custompurified by silica gel chromatography
  8. washeluting with 2-20% methanol in methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-a1636b72dbbb4e759fb21ee6267195f9
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394795B2

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