Hydrochloric Acid → HCID 178479526, Verbindung

HRID 746036Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 746036
C(=O)(O)O.[NH2:5][NH:6][C:7]([NH2:9])=[NH:8].Cl.[Cl:11][C:12]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][CH:17]=[C:16]([Cl:23])[C:13]=1[CH:14]=O>O.C(O)C>[ClH:11].[Cl:11][C:12]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][CH:17]=[C:16]([Cl:23])[C:13]=1[CH:14]=[N:5][NH:6][C:7]([NH2:9])=[NH:8]

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 27949122,6-Dichloro-3-nitrobenzaldehydeHCID 178513185HCID 178513185, Verbindung

Produkt 1

HCID 178479526HCID 178479526, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Aminoguanidine hydrogen carbonate (1.24 g, 9.1 mmol) was added to a solution of concentrated hydrochloric acid (0.8 cm3, 9.3 mmol) in water (3 cm3). After diluting the resulting solution with ethanol (20 cm3), 2,6-dichloro-3-nitrobenzaldehyde (2.0 g, 9.1 mmol) was added and the mixture heated under reflux for 7 h. The solution was evaporated under reduced pressure and the residual solid suspended in refluxing ethanol, basified (pH 11) by addition of dilute sodium hydroxide solution and cooled to yield a white solid which was collected. This solid was dissolved in hot methanol and the solution acidified (pH 2) with ethanolic hydrogen chloride, diluted with diethyl ether and cooled to yield (2,6-dichloro-3-nitrobenzylideneamino)-guanidine hydrochloride as a white solid, m.p. 186°-7° C.

Aufarbeitung

  1. additionwas added
  2. temperaturethe mixture heated
  3. temperatureunder reflux for 7 h
  4. customThe solution was evaporated under reduced pressure
  5. temperaturein refluxing ethanol
  6. additionby addition of dilute sodium hydroxide solution
  7. temperaturecooled
  8. customto yield a white solid which
  9. customwas collected
  10. dissolutionThis solid was dissolved in hot methanol
  11. additiondiluted with diethyl ether
  12. temperaturecooled

Quellen und Nachweise

ORD-Eintrag
ord-65cb7e0178344999b0b2991617e698d7
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04602041

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