関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Hydroxyquinoline | HCID 11376 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-Bromoquinolin-3-ol | HCID 12958744 | — |
反応手順
6.0 mg (41 mmol) of 3-hydroxyquinoline are dissolved in 50 ml of 10% strength sodium hydroxide solution, giving a yellowish brown color. The reaction mixture is cooled to -5° C. using an ice/common salt mixture. A mixture comprising 6.6 g (2.1 ml, 41 mmol) of bromine dissolved in 50 ml of 10% strength sodium hydroxide solution is added dropwise to this solution over a period of 1 hour. During this the temperature of the reaction solution must never exceed 0° C. After this time, the cooling is removed and the reaction solution is stirred at room temperature for another 3 hours. The reaction solution is then cooled to -10° C. The reaction solution cooled to -10° C. [sic]. The reaction solution is then brought to a pH of 3 with 2N hydrochloric acid, during which the temperature of the reaction solution must never exceed -5° to 0° C. This gives the crude product as a light yellow solid. The crude product is recrystallized from 180 ml of ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05266700 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-c0d2322f3d3a49da8ecf7609cbfaa5c3 |
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| 出典メモ | uspto-grants-1993_11 |
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