Reaktion #63194

Reaktionsgleichung

Hydrazine hydrate

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

→

compound

Ausbeute 62.6%

3-Amino-2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-5-(pyrid-3-ylmethyl)pyridine

Ausbeute 62.6%

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe solution was stirred for a further 30 minutes
2. 2
   Sonstigethe catalyst was removed by filtration
3. 3
   Einengenthe filtrate was concentrated to dryness in vacuo
4. 4
   SonstigeThe residue was chromatographed on silica
5. 5
   Wascheneluted with 5% v/v methanol in chloroform
6. 6
   Sonstigerecrystallized from acetonitrile

Vorschrift

Hydrazine hydrate (5 ml) in methanol (25 ml) was added with stirring over 20 minutes to a cooled (10° C.) solution of 2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine (4.75 g) in methanol (250 ml) containing Raney Nickel (ca. 3 g). The solution was stirred for a further 30 minutes, the catalyst was removed by filtration and the filtrate was concentrated to dryness in vacuo. The residue was chromatographed on silica eluted with 5% v/v methanol in chloroform and then recrystallized from acetonitrile to give the tile compound (2.78 g), m.p. 85°-87° C.

Quelle