HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrazine hydrate (1:1) → 3-Amino-2-[4-(5-bromo-3-methylpyrid-2-yl)-butylamino]-5-(pyrid-3-ylmethyl)pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Edukt | 2-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine | HCID 19851793 | — |
| Katalysator | Nickel | HCID 935 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 3-Amino-2-[4-(5-bromo-3-methylpyrid-2-yl)-butylamino]-5-(pyrid-3-ylmethyl)pyridine | HCID 19851789 | 62,6% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04764519 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-1b8aae2df5184c04a17fff473013080f |
| Quellennotiz | uspto-grants-1988_08 |