Trimethylamine → N,N-dimethyl-5-nitropyridin-2-amine

HRID 865668

Reaktionsgleichung

Reaktionsgleichung von HRID 865668
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[CH3:11][N:12](C)[CH3:13]>CCO>[CH3:11][N:12]([CH3:13])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1

Komponenten

4

Edukt 2

HCID 1146TrimethylamineHCID 783082-Chloro-5-nitropyridine

Produkt 1

HCID 75707N,N-dimethyl-5-nitropyridin-2-amineAusbeute 89,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A mechanically stirred mixture of 2-chloro-5-nitropyridine (56.25 g, 0.355 mol) and absolute EtOH (960 ml), under nitrogen was treated, during 15 minutes with 25% aqueous trimethylamine (217 g). The mixture warmed to 40° C. and a thick yellow precipitate formed; it was warmed to 80° C. during 1 hour, cooled to ambient temperature and filtered. The solid was washed with cold 20% H2O-EtOH and dried to give 53.2 g of the titled product, m.p. 151°-152° C.

Aufarbeitung

  1. customa thick yellow precipitate formed
  2. temperatureit was warmed to 80° C. during 1 hour
  3. temperaturecooled to ambient temperature
  4. filtrationfiltered
  5. washThe solid was washed with cold 20% H2O-EtOH
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a42ee2f1e2da43618bd597d4a0e3c400
Quelldatensatz
uspto-grants-1996_10
Patentnummer
US05567722

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