関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium hypobromite | HCID 23673712 | — |
| 反応物 | HCID 178418543 | HCID 178418543 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178418525 | HCID 178418525 | 63.5% |
反応手順
To a solution of 10 g (0.07 mole) of 2-hydroxy-nicotinic acid in 16.8 g of 50% sodium hydroxide (0.21 mole) diluted with 25 ml of water was added 200 ml of sodium hypobromite solution prepared by adding 13.6 g (0.17 mole) of bromine to a solution of 20.16 g of 50% sodium hydroxide (0.25 mole) in 125 ml of water at 0° C. diluted to 400 ml. After 24 hrs of stirring at room temperature, another 100 ml portion of the above sodium hypobromite solution was added and the reaction solution was stirred for another 24 hr. The reaction solution was cooled in an ice bath and acidified carefully with 12N hydrochloric acid. Crystallization from isopropyl alcohol gave 9.7 g (63.5%) of product. A sample was further recrystallized from 95% ethanol, m.p. 245° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04727152 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-f3db1044f1d24b8cbe93aa3f0f632b1b |
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| 出典メモ | uspto-grants-1988_02 |
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