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Hydrazine hydrate (1:1) → 3-Amino-2-[4-(5-bromo-3-methylpyrid-2-yl)-butylamino]-5-(pyrid-3-ylmethyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine | HCID 19851793 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Amino-2-[4-(5-bromo-3-methylpyrid-2-yl)-butylamino]-5-(pyrid-3-ylmethyl)pyridine | HCID 19851789 | 62.6% |
反応手順
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 recrystallised from acetonitrile to give the title compound (2.78 g), m.p. 85°-87° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04863933 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-5951a9426b2c402fb309cc3cf73eb3ac |
| 出典メモ | uspto-grants-1989_09 |