Reaktionsgleichung
O.NN.[Br:4][C:5]1[CH:6]=[C:7]([CH3:31])[C:8]([CH2:11][CH2:12][CH2:13][NH:14][C:15]2[C:20]([N+:21]([O-])=O)=[CH:19][C:18]([CH2:24][C:25]3[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=3)=[CH:17][N:16]=2)=[N:9][CH:10]=1>[Ni].CO.C(O)C>[Br:4][C:5]1[CH:6]=[C:7]([CH3:31])[C:8]([CH2:11][CH2:12][CH2:13][NH:14][C:15]2[C:20]([NH2:21])=[CH:19][C:18]([CH2:24][C:25]3[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=3)=[CH:17][N:16]=2)=[N:9][CH:10]=1Komponenten
6
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
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.
Aufarbeitung
- customat 5°-10° C
- customReaction
- stirringto stir at 5° C. for a further 45 minutes
- filtrationRaney nickel was filtered off
- concentrationthe filtrate was concentrated to dryness
- customto give an oil which
- customwas re-evaporated with n-propanol giving the title compound, theoretical yield, crude product
- customused directly in next reaction
Quellen und Nachweise
- ORD-Eintrag
- ord-24e22c8f9dcf4485aa3c784a45c563a5
- Quelldatensatz
- uspto-grants-1988_08
- Patentnummer
- US04764519
Verknüpfte Notizen
Wird geladen…