関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nicotinamide | HCID 936 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 3-Aminocarbonyl-2-chloro-6-methyl-4-(trifluoromethyl)pyridine | HCID 19960052 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Amino-2-chloro-6-methyl-4-(trifluoromethyl)pyridine | HCID 19960079 | — |
反応手順
To a solution of 6.6 g of sodium hydroxide in 60 ml of water at 5° C. was added 9.3 g of bromine. When a clear solution was obtained, 9.2 g of 3-aminocarbonyl-2-chloro-6-methyl-4-(trifluoromethyl)pyridine was added quickly, maintaining the temperature below 5° C. The resulting mixture was stirred until the 3-(aminocarbonyl)pyridine dissolved (~30 min). The cooling bath was removed and the mixture was then warmed to 75° C. for 30 min. After cooling to room temperature, the 3-aminopyridine product was extracted with ethyl acetate, dried (magnesium sulfate), filtered, and evaporated to give 4.9 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05366972 |
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| 出典データセット | uspto-grants-1994_11 |
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| ORD ID | ord-a33ee7b2f5c043f4b4ff964f9cdfa645 |
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| 出典メモ | uspto-grants-1994_11 |
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