Water → HCID 178434678, Verbindung

HRID 17831

Reaktionsgleichung

Reaktionsgleichung von HRID 17831
O.[NH2:2][NH2:3].C(O[C:7](=[C:9]([C:12]#[N:13])[C:10]#[N:11])[CH3:8])C.O>CCO>[NH2:11][C:10]1[NH:3][N:2]=[C:7]([CH3:8])[C:9]=1[C:12]#[N:13]

Komponenten

5

Edukt 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 79450(1-Ethoxyethylidene)malononitrile

Produkt 1

HCID 178434678HCID 178434678, VerbindungAusbeute 71,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

Hydrazine monohydrate (6.8 ml, 0.14 mol) was dissolved in EtOH (10 ml) and cooled to 0° C. (1-Ethoxyethylidene)malononitrile (10 g, 0.073 mol) was added slowly and the mixture was heated at 95° C. for 2 h. After cooling to rt, water (20 ml) was added and the mixture was allowed to stand at rt overnight. The mixture was concentrated under reduced pressure and the resulting residue treated with EtOH (6 ml) and water (6 ml). After cooling in an ice/water bath for 10 min, the resulting precipitate was collected by filtration to give 6.34 g of 5-amino-3-methyl-1H-pyrazole-4-carbonitrile.

Aufarbeitung

  1. additionwas added slowly
  2. temperatureAfter cooling to rt
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionthe resulting residue treated with EtOH (6 ml) and water (6 ml)
  5. temperatureAfter cooling in an ice/water bath for 10 min
  6. filtrationthe resulting precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-d69380414ccc4fa79cd8e846802ba5e2
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741318B2

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