関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Potassium sodium tartarate | HCID 9855836 | — |
| 反応物 | Diethyl 4-bromophenylmalonate | HCID 10519382 | — |
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(4-Bromophenyl)propane-1,3-diol | HCID 21866701 | 37.4% |
反応手順
To a solution of diethyl 2-(4-bromophenyl)malonate (18.1 g, 57.5 mmol) in ether (285 ml) was added 0.98M-diisobutylaluminium hydride in hexane (259 ml, 254 mmol) at 0° C. under nitrogen atmosphere. The resulting mixture was stirred at 0° C. for 4 hours. Aqueous potassium sodium tartrate (0.57M, 500 ml) was added to the reaction mixture for quenching the aluminum reagent and the mixture was stirred for 14 hours. The organic layer was extracted with ethyl acetate and dried over sodium sulfate. After concentration, the residue was purified by silica gel column chromatography (eluant: hexane/ethyl acetate=40/60 to ethyl acetate only) to afford 2-(4-bromophenyl)propane-1,3-diol as white solid (4.97 g, 37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09108957B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-073ca934b9104bed9e97062c70542276 |
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| 出典メモ | uspto-grants-2015_08 |
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