関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Ethyl Bromide | HCID 6332 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Acetopiperone | HCID 76622 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[3,4-(Methylenedioxy)phenyl]-2-butanol | HCID 19001698 | 95.9% |
反応手順
15 ml of tetrahydrofuran and a catalytic amount of iodine were added to 340 mg of magnesium ribbon to obtain a mixture. 1.59 g of bromoethane was gradually added to the mixture in a stream of nitrogen in such a way that the reaction system was mildly refluxed. The resulting mixture was heated under reflux for 30 minutes and cooled, followed by the addition of a solution of 2 g of 5 -acetyl-1,3-benzodioxole in tetrahydrofuran. The obtained mixture was stirred at a room temperature for 20 minutes, followed by the addition of a saturated aqueous solution of ammonium chloride and water. The obtained mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of common salt, dried over ahydrous magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. 2.27 g of the title compound was obtained as a crude oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05475024 |
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| 出典データセット | uspto-grants-1995_12 |
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| ORD ID | ord-1668fad0a7184ee29c1e47d2edd15a0c |
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| 出典メモ | uspto-grants-1995_12 |
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