関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | 6-Chloroquinaldine | HCID 135965 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 6-Chloro-2-methyl-5-nitroquinoline | HCID 15571772 | 89.2% |
反応手順
6-Chloroquinaldine (11 g) was dissolved in 15 ml of concentrated sulfuric acid and the solution was ice-cooled. Then, a solution of 7.1 g of potassium nitrate dissolved in 20 ml of concentrated sulfuric acid was added to the solution dropwise, during which operation the reaction temperature was maintained at 10° C. or less. After completion of addition the mixture was agitated at the same temperature as above for 1 hour and then poured onto 200 g of ice. Subsequently, the mixture was rendered alkaline with 10% sodium hydroxide, taking care that the internal temperature should not be raised to above 20° C., thus forming a pale yellow precipitate. The precipitate was collected by filtration, washed with water and recrystallized from ethanol to obtain 12.3 g of 5-nitro-6-chloroquinaldine as pale yellow rhombic crystals having a melting point of 123° to 124° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04416884 |
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| 出典データセット | uspto-grants-1983_11 |
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| ORD ID | ord-b34afdba5e95464583f932dd7345f107 |
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| 出典メモ | uspto-grants-1983_11 |
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