関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 4-Methylbenzaldehyde | HCID 7725 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Chloro-6-hydroxyacetophenone | HCID 74061 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-chloro-3-hydroxy-2-(4-methylphenyl)-4H-1-benzopyran-4-one | HCID 7746661 | — |
反応手順
A 8.5 g quantity of 5'-chloro-2'-hydroxyacetophenone and 6.0 g of p-tolualdehyde were dissolved in 105 ml of ethanol. Then 17 ml of an aqueous solution containing 10 g of sodium hydroxide was slowly added thereto dropwise and stirred at room temperature for 4 hours. Then 350 ml of ethanol and 17 ml of an aqueous solution containing 3.5 g of sodium hydroxide were added to the reaction mixture, and 8.3 ml of a 30% aqueous hydrogen peroxide solution was further added dropwise slowly and stirred at room temperature for 12 hours. A 10% aqueous HCl solution was added to adjust the reaction mixture to pH 3. The crystals precipitated were collected by filtration and washed serially with 10 ml of water, 5 ml of ethanol and 10 ml of diethyl ether, thus giving 6.0 g of 6-chloro-3-hydroxy-2-(4-methylphenyl)-4H-1-benzopyran-4-one as crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05527786 |
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| 出典データセット | uspto-grants-1996_06 |
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| ORD ID | ord-1c3de887f27a413d90130333a19f58ab |
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| 出典メモ | uspto-grants-1996_06 |
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