関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 2-Methyl-3,4,6-trifluorobenzoyl chloride | HCID 15007607 | — |
| 触媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate | HCID 17879412 | — |
反応手順
Separately, two drops of carbon tetrachloride are added to a solution of metallic magnesium (0.4 g) in absolute ethanol (0.9 ml). When the reaction starts, a mixture of diethyl malonate (2.6 ml), absolute ethanol (1.6 ml) and anhydrous toluene (6 ml) is added dropwise below 60° C. After stirring at 60° C. for 1 hour, the reaction mixture is cooled to 0° C. and thereto a solution of 2-methyl-3,4,6-trifluorobenzoyl chloride prepared above in toluene (5 ml) is added dropwise. After stirring for 30 minutes, a mixture of conc. sulfuric acid (0.4 ml) and water (6 ml) is added and the mixture is extracted with diethyl ether, and the extract is dried over magnesium sulfate and concentrated to give diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate (5.2 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05723648 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-2c7533e52831442a89bfed399496e97e |
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| 出典メモ | uspto-grants-1998_03 |
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