Hydrazine hydrate (1:1) → HCID 12297944, Verbindung

HRID 1730643Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1730643
[NH2:1][C:2]1[N:12]=[C:11]([CH3:13])[C:10]([NH:14][C:15](=[O:17])[CH3:16])=[C:9]([CH3:18])[C:3]=1[C:4](OCC)=[O:5].O.[NH2:20][NH2:21]>O.CO>[NH2:1][C:2]1[N:12]=[C:11]([CH3:13])[C:10]([NH:14][C:15](=[O:17])[CH3:16])=[C:9]([CH3:18])[C:3]=1[C:4]([NH:20][NH2:21])=[O:5]

Komponenten

5

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 12297943HCID 12297943, Verbindung

Produkt 1

HCID 12297944HCID 12297944, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of ethyl 2-amino-5-acetamido-4,6-dimethylnicotinate (45.3 g., 0.18 mole) and hydrazine hydrate (100 ml.) is heated in an oil bath with stirring at 120° C. for two hours. The mixture is cooled, the solid collected, and a second crop of solid obtained by evaporating the mother liquor to about half its initial volume. The combined solids melt at 293° C. (dec.), yield 38.1 g. (89%). Analytically pure compound is obtained by dissolving the solid in about six and one-half parts (volume by weight) of hot water and diluting the filtered solution with methanol. The purified product decomposed at about 309° C. with only partial melting.

Aufarbeitung

  1. temperatureis heated in an oil bath
  2. temperatureThe mixture is cooled
  3. customthe solid collected
  4. customa second crop of solid obtained
  5. customby evaporating the mother liquor to about half its initial volume
  6. customAnalytically pure compound is obtained
  7. customdecomposed at about 309° C. with only partial melting

Quellen und Nachweise

ORD-Eintrag
ord-61250c22e6cd452f97f736c68fb8666a
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03993656

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