関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | Methyl 2-(2-methoxy-2-oxoethyl)thiophene-3-carboxylate | HCID 58952963 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(3-Hydroxymethylthiophen-2-yl)ethanol | HCID 11182761 | 87% |
反応手順
In a dried vessel, 600 mg of lithium aluminum hydride was charged under a nitrogen atmosphere, and then 26 mL of anhydrous tetrahydrofuran was added thereto. To the resulting suspension, a solution of 2.8 g of the compound obtained in Example 1 dissolved in 10 mL of tetrahydrofuran was added over about 5 minutes. The resulting mixture was stirred at room temperature for 1 hour, and then refluxed for 1 hour. The reaction solution was cooled to 0° C., and 0.5 mL of water, 0.5 mL of 15% sodium hydroxide aqueous solution, and 4 mL of water were added thereto slowly in succession. The resulting mixture was stirred for about 1 hour, and the insoluble materials was filtered and washed with 30 mL of tetrahydrofuran. Combined filtrate was concentrated by evaporation under reduced pressure to obtain 1.8 g (yield of 87%) of oily title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449580B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-2cdc5d8640f14ccdbca4f7b166295c52 |
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| 出典メモ | uspto-grants-2008_11 |
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