関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-4'-nitroacetophenone | HCID 66840 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 2-(4-Nitrophenyl)oxirane | HCID 92228 | 100% |
反応手順
To an ice-cold stirred suspension of 4-nitrophenacyl bromide (80 g, 0.33 mol) in methanol (800 mL) was added sodium borohydride (13.64 g, 0.36 mol) in small portions. After stirring for 2 h at 0-5° C., potassium carbonate (45.20 g, 0.33 mol) was added in small portions at the same temperature. The suspension was stirred for 18 h at room temperature, diluted with brine (600 mL) and extracted with diethyl ether (600 mL, 500 mL), the combined organic layers were dried over sodium sulfate, filtered and evaporated. The title compound (54.87 g, 0.33 mmol, 100%) was obtained as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08372970B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-ce75885e707e433d8f5ee23e443ec10f |
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| 出典メモ | uspto-grants-2013_02 |
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