関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | N-(4-methoxyphenyl)pyridin-4-amine | HCID 3628677 | — |
| 溶媒 | Hydrogen Bromide | HCID 260 | — |
| 生成物 | 4-[(Pyridin-4-yl)amino]phenol | HCID 13098456 | — |
反応手順
A mixture of the product from step (i) above (2.0 g) and 48% w/v hydrobromic acid (30 ml) was heated at 140° C. for 4 hours. The cooled solution was neutralised with 0.880 ammonia solution and then extracted four times with ethyl acetate. The combined organic extracts were washed with water and saturated sodium chloride solution, then dried (MgSO4) and evaporated. Purification by flash chromatography on silica, eluting with 10 to 20% v/v methanol/dichloromethane gave 4-(4-pyridylamino)phenol, 0.78 g as an off-white solid: m.p. 246°-248° C.; NMR (CDCl3 +d6DMSO) δ 8.92 (1H, b), 8.09 (2H, d), 7.31 (1H, s), 7.00 (2H, d), 6.79 (2H, d), 6.67 (2H, dd); m/e 187 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05652242 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-a737062066b54e3481095b72f2073ca3 |
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| 出典メモ | uspto-grants-1997_07 |
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