関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-2-methyl-1-propene | HCID 357785 | — |
| 反応物 | N-(2-Bromo-5-nitrophenyl)acetamide | HCID 21959509 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(2-bromo-5-nitrophenyl)-N-(2-methylprop-2-en-1-yl)acetamide | HCID 21959573 | 85% |
反応手順
At 25° C., a solution of 3-bromo-2-methylpropene (3.4 g, 55.6 mmol) in anhydrous DMF (30 mL) was added dropwise to a solution of N-(2-bromo-5-nitrophenyl)acetamide (3.6 g, 13.9 mmol) and potassium carbonate (3.9 g, 27.8 mmol) in anhydrous DMF (50 mL). The reaction mixture was stirred at 25° C. overnight. The reaction mixture was then filtered and the filtrate was treated with sat. Na2CO3 solution. The organic layer was separated and the aqueous layer was extracted with EtOAc. The combined organic extracts were washed with water and brine, dried over MgSO4, filtered and concentrated under vacuum to provide N-(2-bromo-5-nitrophenyl)-N-(2-methylprop-2-enyl)acetamide as a golden solid (3.1 g, 85%). ESI-MS 313 m/z (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829204B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-252a44ef5fe044feb5c56887c93dee3d |
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| 出典メモ | uspto-grants-2014_09 |
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