반응 #63208

반응 방정식

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

용매

methanol

ethanol

반응 조건

후처리

1. 1
   기타at 5°-10° C
2. 2
   기타Reaction
3. 3
   workup.STIRRINGto stir at 5° C. for a further 45 minutes
4. 4
   여과Raney nickel was filtered off
5. 5
   농축the filtrate was concentrated to dryness
6. 6
   기타to give an oil which
7. 7
   기타was re-evaporated with n-propanol giving the title compound, theoretical yield, crude product
8. 8
   기타used directly in next reaction

실험 절차

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.

출처