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Hydrochloric Acid → HCID 19012219, Verbindung

HRID 2397587
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2397587
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([CH3:11])[C:5]([N+:12]([O-])=O)=[C:4]([CH3:15])[N:3]=1.C(O)C.[H][H].Cl>[Pd].C.C(O)(C)C>[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([CH3:11])[C:5]([NH2:12])=[C:4]([CH3:15])[N:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 197540694,6-Dimethyl-3,5-dinitropyridin-2-amineHCID 178418361HCID 178418361, Verbindung2×

Produkt 1

HCID 19012219HCID 19012219, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14818447
Palladiumcarbon
Katalysator
HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A 500 ml Parr Bottle was charged with 2-amino-4,6-dimethyl-3,5-dinitropyridine (21.2 g, 0.10 mole), 250 ml absolute ethanol, and 20 g 5% Pd/charcoal catalyst. The mixture was subjected to hydrogenation at ambient temperature with an initial hydrogen pressure of 60 psig. When no further uptake of hydrogen was observed, the mixture was filtered free of catalyst under a nitrogen atmosphere, and concentrated under vacuum to a volume of about 100 ml. The product concentrate was treated, under nitrogen at ice temperature, with a cold solution of hydrogen chloride (0.5 mole) in 85 ml anhydrous isopropyl alcohol. The trihydrochloride salt of 2,3,5-triamino-4,6-dimethylpyridine was obtained after vigorous stirring, filtering under nitrogen, and vacuum drying under high vacuum over P2O5 at 80°-90° C.

Aufarbeitung

  1. filtrationthe mixture was filtered free of catalyst under a nitrogen atmosphere
  2. concentrationconcentrated under vacuum to a volume of about 100 ml
  3. concentrationThe product concentrate

Quellen und Nachweise

ORD-Eintrag
ord-2a56b0bd65d64252a834100e2697cee7
Quelldatensatz
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04022793

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