関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 5-Amino-2-(3-aminopropyl)-3-methylpyridine | HCID 19851780 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Aminopropyl)-5-bromo-3-methylpyridine | HCID 19851781 | — |
反応手順
5-Amino-2-(3-aminopropyl)-3-methylpyridine (8.05 g) in hydrobromic acid (48%, 75 ml) and water (8 ml) wasreacted with cuprous bromide (8.73 g) and copper bronze (0.29 g). A solution of sodium nitrite (5.1 g) in water (8 ml) was added at 5°-8° C. over 40 minutes, the reaction mixture was allowed to stir at 5°-8° C. for one hour and then stirred at room temperature for 3 hours. The cooled reaction mixture was then basified with ammonium hydroxide (70 ml), which was then extracted with chloroform 3×150 ml. The chloroform extracts were then washed with fresh ammonium hydroxide and water (70 ml of each) till no more blue colour was visible in the aqueous layer. Chloroform extracts were dried over magnesium sulphate, filtered and concentrated to dryness to give the title compound (8.2 g) as an amber oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04764519 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-9465c95b41ee425b9b6a12fd598f2ebc |
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| 出典メモ | uspto-grants-1988_08 |
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