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Water → Benzamide, N-(4-fluoro-3-nitrophenyl)-N-methyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | N-(4-fluoro-3-nitrophenyl)benzamide | HCID 3535228 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzamide, N-(4-fluoro-3-nitrophenyl)-N-methyl- | HCID 11460004 | — |
反応手順
To a solution of N-(4-fluoro-3-nitro-phenyl)-benzamide (1.60 g, 6.15 mmol) in anhydrous DMF was added iodomethane (3.49 g, 24.60 mmol, 1.53 ml) under argon. 60% Sodium hydride (0.37 g, 9.23 mmol) was then added portionwise to the cooled solution (0° C.) and the reaction mixture was then stirred at room temperature for 24 h. The solution was poured slowly into water and the aqueous layer was extracted 3× with ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate and the solvent was removed under reduced pressure. The residue was purified by flash chromatography, eluting with hexane/ethyl acetate (4:1) to give N-(4-fluoro-3-nitro-phenyl)-N-methyl-benzamide. (1.47 g, 87%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07138420B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-e80efaf38bfa4c289894f176ae48ca8d |
| 出典メモ | uspto-grants-2006_11 |