関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Methoxybenzaldehyde | HCID 31244 | — |
| 反応物 | 4,6-Dimethyl-7-hydroxy-1-indanone | HCID 240718 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,3-dihydro-4,6-dimethyl-7-hydroxy-2-(4-methoxybenzylidene)-1H-inden-1-one | HCID 54463546 | — |
反応手順
10 Grams of 2,3-dihydro-4,6dimethyl-7-hydroxy-1H-inden-1-one was dissolved in 200 ml of dimethylformamide, then 5.45 g of 60%-sodium hydride was added gradually thereto and the reaction mixture was stirred at room temperature for 30 minutes. Next, 6.91 ml of p-anisaldehyde was added to the reaction mixture and further stirred at room temperature for 1 hour. The reaction mixture was poured into 500 ml of ice-water, then acidified by adding hydrochloric acid, and the crystals formed were collected by filtration. The crystals were washed with water and with n-hexane and dried. Recrystallized from ethanol to obtain 16.09 g of 2,3-dihydro-4,6-dimethyl-7-hydroxy-2-(4-methoxybenzylidene)-1H-inden-1-one. Yellow needle-like crystals. Melting point: 192°-193° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05242919 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-6737505c6dd04f6cbd916f255e400141 |
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| 出典メモ | uspto-grants-1993_09 |
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