関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium sulfate decahydrate | HCID 62649 | — |
| 反応物 | Ethyl 3-(2-methoxyphenyl)prop-2-enoate | HCID 90485 | — |
| 反応物 | Hydride | HCID 166653 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(2-Methoxy-phenyl)-propan-1-ol | HCID 254958 | 81% |
反応手順
A solution of 980 mg of ethyl 2-methoxycinnamate in 15 ml of tetrahydrofuran was added dropwise to a dispersion of 290 mg of lithium aluminum hydride and 10 ml of tetrahydrofuran, whilst ice-cooling. After the addition was complete, the reaction mixture was stirred at room temperature for 1.5 hours, and then sufficient sodium sulfate decahydrate was slowly added, whilst ice-cooling, to the mixture in order to decompose any excess of the hydride. Insoluble materials were filtered off, and the filtrate was concentrated by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using a 3:1 by volume mixture of hexane and ethyl acetate as the eluent, to give 640 mg of 3-(2-methoxyphenyl)propanol as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05556864 |
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| 出典データセット | uspto-grants-1996_09 |
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| ORD ID | ord-88cc5d468bbc4a44826ea7d8588e3aeb |
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| 出典メモ | uspto-grants-1996_09 |
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