Reaktion #63193

Reaktionsgleichung

4-(5-bromo-3-methylpyrid-2-yl)butylamine

2-chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride

→

title compound

2-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in water (100 ml)
3. 3
   Extraktionextracted with chloroform (100 ml)
4. 4
   ExtraktionThe chloroform extract
5. 5
   Sonstigewas chromatographed on silica
6. 6
   Wascheneluted with 5% v/v methanol in chloroform
7. 7
   Sonstigefollowed by recrystallisation from chloroform/hexane

Vorschrift

A mixture of 4-(5-bromo-3-methylpyrid-2-yl)butylamine (11.79 g) and 2-chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride (4.57 g) was refluxed in ethanol (100 ml) for 8 hours. The solvent was removed in vacuo, the residue was dissolved in water (100 ml) and then extracted with chloroform (100 ml). The chloroform extract was chromatographed on silica eluted with 5% v/v methanol in chloroform followed by recrystallisation from chloroform/hexane to give the title compound as a yellow solid, m.p. 82°-84° C.

Quelle