Hydrazine hydrate (1:1) → 5-Cyano-2-hydrazino-4-methylamino-pyrimidine

HRID 1586404Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1586404
[C:1]([C:3]1[C:4]([NH:11][CH3:12])=[N:5][C:6](SC)=[N:7][CH:8]=1)#[N:2].O.[NH2:14][NH2:15]>C(O)C>[C:1]([C:3]1[C:4]([NH:11][CH3:12])=[N:5][C:6]([NH:14][NH2:15])=[N:7][CH:8]=1)#[N:2]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 106789344-(Methylamino)-2-(methylthio)pyrimidine-5-carbonitrile

Produkt 1

HCID 218527585-Cyano-2-hydrazino-4-methylamino-pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 5-cyano-4-methylamino-2-methylsulfanyl-pyrimidine (25.86 g) from Example 3 and hydrazine hydrate (52 mL) in ethanol (250 mL) was heated at reflux with stirring for 3 hours. The reaction mixture was cooled to room temperature and the insoluble product was collected by filtration, washed with cold aqueous ethanol (1:1) to give 23 g of the title compound. Crystallization from ethanol afforded an analytically pure sample of 5-cyano-2-hydrazino-4-methylamino-pyrimidine; mp 247-249° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux
  3. filtrationthe insoluble product was collected by filtration
  4. washwashed with cold aqueous ethanol (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-ed3f60ed5811407d9d82a3513081be99
Quelldatensatz
uspto-grants-1999_08
Patentnummer
US05945422

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