関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Bromobenzonitrile | HCID 23381 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Bromobenzamide | HCID 89807 | 80% |
反応手順
To a solution of 3-bromobenzonitrile (0.91 g, 5 mmol) in dioxane (19 mL), NaBO3.4H2O (2.12 g, 13.78 mmol) and H2O (19 mL) were added. The mixture was stirred at 80° C. 16 hours (h), cooled, added of H2O and extracted with CH2Cl2. The combined organic layers were dried over Na2SO4 and evaporated. Purification of the residue by column chromatography (hexane/EtOAc 2:8) and recrystallization gave the desired product as colorless tablets. Yield 80% (EtOH). Mp: 156–7° C. (lit. 156° C.) (Pearson, D. E. et al., J. Org. Chem., 28: 3147–3149, (1963)). MS (EI): m/z 199 (M+); 183 (100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176201B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-e1cdeceb7dc34f52869aa74648684cc2 |
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| 出典メモ | uspto-grants-2007_02 |
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