Histamine → HCID 178526675, Verbindung

HRID 744047

Reaktionsgleichung

Reaktionsgleichung von HRID 744047
[CH:1]1[N:5]=[CH:4][NH:3][C:2]=1[CH2:6][CH2:7][NH2:8].Cl[C:10]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][CH:13]=[CH:12][N:11]=1>CC(O)C>[NH:5]1[CH:1]=[C:2]([CH2:6][CH2:7][NH:8][C:10]2[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][CH:13]=[CH:12][N:11]=2)[N:3]=[CH:4]1

Komponenten

4

Edukt 2

HCID 774HistamineHCID 796132-Chloro-3-nitropyridine

Produkt 1

HCID 178526675HCID 178526675, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

1.14 g (10.2 mmol) of histamine base and 1.62 g (10.2 mmol) of 2-chloro-3-nitropyridine are brought to reflux in 5 ml of 2-propanol for 3 h. Evaporation of the solvent under reduced pressure and purification of the solid residue by chromatography on a column of silica gel, eluted with chloroform containing increasing amounts of methanol (5, 10 and 20%), provide the title compound. M.p.: 178°-180° C. (yield 65%; ethanol:water).

Aufarbeitung

  1. customEvaporation of the solvent
  2. customunder reduced pressure and purification of the solid residue by chromatography on a column of silica gel
  3. washeluted with chloroform containing
  4. temperatureincreasing amounts of methanol (5, 10 and 20%)

Quellen und Nachweise

ORD-Eintrag
ord-82a4e4fab68b49b09087fd77473ed05a
Quelldatensatz
uspto-grants-1996_09
Patentnummer
US05559113

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