関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Ammonium Bromide | HCID 25514 | — |
| 反応物 | Sodium metaborate | HCID 145326 | — |
| 反応物 | 1-(6-Methylpyridin-3-yl)butane-1,3-dione | HCID 20212814 | — |
| 反応物 | 1-(2-Methyl-5-pyridyl)-3-amino-n-butanol | HCID 54430743 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(2-Methyl-5-pyridyl)-3-amino-but-2-en-1-one | HCID 68135972 | — |
反応手順
1-(2-Methyl-5-pyridyl)-3-amino-n-butanol can be used as the starting material, is obtained as follows: 20.0 g of (6-methyl-nicotinoyl)-acetone, 200 ml of ethanol and 0.5 g of ammonium bromide are saturated with ammonia at 50° and heated at 50° for 15 hours whilst continuing to introduce ammonia. 8.5 g of sodium boranate are introduced in portions over the course of 1 hour into the solution, obtained above, of 1-(2-methyl-5-pyridyl)-3-amino-but-2-en-1-one of the formula ##EQU46## and the mixture is stirred for 7 hours at 70° . The solvent is distilled off in vacuo and the residue is taken up in 20% strength aqueous potassium hydroxide solution and pentanol-1. After working up in the usual manner, 19.2 g of crude 1-(2-methyl-5-pyridyl)-3-amino-n-butanol of the formula ##EQU47## are obtained from the pentanol solution as an oil which can be purified further by column chromatography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03969363 |
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| 出典データセット | uspto-grants-1976_07 |
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| ORD ID | ord-33b53f02418b48518ef71bac0104e40a |
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| 出典メモ | uspto-grants-1976_07 |
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