関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium sulfate decahydrate | HCID 62649 | — |
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 反応物 | Ethyl 1-(4-fluorophenyl)imidazole-5-carboxylate | HCID 55563221 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [1-(4-fluorophenyl)-1H-imidazol-5-yl]methanol | HCID 69209067 | 53.3% |
反応手順
To a solution of ethyl 1-(4-fluorophenyl)-1H-imidazole-5-carboxylate (9.37 g) in tetrahydrofuran (100 ml) was added dropwise diisobutylaluminum hydride (1.5 mol/l toluene solution, 60 ml) at 0° C. The mixture was stirred at 0° C. for 1 hr., sodium sulfate decahydrate (13.0 g) was added and the mixture was stirred at room temperature for 1 hr. The reaction mixture was filtered, and the organic layer was concentrated to give [1-(4-fluorophenyl)-1H-imidazol-5-yl]methanol (4.10 g, 53%) as crystals. Recrystallization thereof from ethyl acetate-isopropyl ether gave pale-yellow prism crystals. melting point: 96-98° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07423159B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-8ba9733e0fdc485da6271498d954698d |
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| 出典メモ | uspto-grants-2008_09 |
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