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1-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine → 5-Amino-2-(4-[4-methoxyphenyl]piperazin-1-yl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine | HCID 3742676 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-Amino-2-(4-[4-methoxyphenyl]piperazin-1-yl)pyridine | HCID 9161650 | — |
反応手順
A suspension of the product of part (i) (4.0 g, 12 mmole) in ethanol (150 ml) was hydrogenated at 45 p.s.i. (310 kPa) over 5% platinum on carbon (0.1 g) for 5 hours. After this time an additional portion of the catalyst (0.1 g) was added and hydrogenation was continued at room temperature for a further 48 hours. The catalyst was removed by filtration and the filtrate concentrated under reduced pressure. The dark residue was purified by flash chromatography on silica gel eluting with ethyl acetate (97):methanol (3) to yield, after collection and evaporation of appropriate fractions, the desired product, m.p. 134°-135° (1.2 g, 33%), which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05023258 |
| 出典データセット | uspto-grants-1991_06 |
| ORD ID | ord-b3d5954149084e71920ccc4ff61ba029 |
| 出典メモ | uspto-grants-1991_06 |