Reaktion #63208

Reaktionsgleichung

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

Hydrazine hydrate

→

2-[3-(5-Bromo-3-methylpyrid-2-yl)-propylamino]-3-amino-5-(pyrid-3-ylmethyl)pyridine

Lösungsmittel

methanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat 5°-10° C
2. 2
   SonstigeReaction
3. 3
   workup.STIRRINGto stir at 5° C. for a further 45 minutes
4. 4
   FiltrationRaney nickel was filtered off
5. 5
   Einengenthe filtrate was concentrated to dryness
6. 6
   Sonstigeto give an oil which
7. 7
   Sonstigewas re-evaporated with n-propanol giving the title compound, theoretical yield, crude product
8. 8
   Sonstigeused directly in next reaction

Vorschrift

Hydrazine hydrate (5.3 ml in 25 ml methanol) was added dropwise over 25 minutes to a stirred and cooled suspension under nitrogen of 2-[3-(5-bromo-3-methylpyrid-2-yl)propylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine (5.07 g) and Raney nickel (10 g) in methanol (600 ml) and ethanol (100 ml) keeping the temperature at 5°-10° C. Reaction was allowed to stir at 5° C. for a further 45 minutes. Raney nickel was filtered off and the filtrate was concentrated to dryness to give an oil which was re-evaporated with n-propanol giving the title compound, theoretical yield, crude product used directly in next reaction.

Quelle