関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-methoxy-1-methyl-1H-indole | HCID 819864 | — |
| 生成物 | 5-methoxy-1-methyl-1H-indole-3-carbaldehyde | HCID 925973 | — |
反応手順
While cooling in order to maintain the temperature of the reaction medium below 15° C., phosphorus oxychloride (9 ml) is added dropwise to 35 ml of dimethylformamide (DMF), and 5-methoxy-1-methylindole (14.1 g), dissolved in DMF (25 ml) is added in a single portion. The resulting heterogeneous mixture is heated to 110° C. for 1 minute, and then maintained at 65° C. for 30 minutes while being stirred mechanically. After the mixture has been allowed to cool, it is decomposed by adding 200 ml of ice-cold water, and then treated with 5N sodium hydroxide solution (100 ml). The precipitate formed is filtered off and recrystallized in ethanol, to give 14.53 g (87.7%) of colorless scales, m.p.=134° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04966971 |
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| 出典データセット | uspto-grants-1990_10 |
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| ORD ID | ord-fcd1736e14204c9a9eeb41b043e7158c |
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| 出典メモ | uspto-grants-1990_10 |
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