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Sodium Chloride → 2-bromo-3-(1,5-dimethyl-1H-indol-3-yl)-N-methylmaleimide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-bromo-3-(5-methyl-1H-indol-3-yl)-N-methylmaleimide | HCID 9883510 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-bromo-3-(1,5-dimethyl-1H-indol-3-yl)-N-methylmaleimide | HCID 18505444 | 96.8% |
反応手順
Potassium carbonate (130 mg, 0.94 mmol) and methyl iodide (0.06 mL, 0.94 mmol) were added under ice cooling to 2-bromo-3-(5-methyl-1H-indol-3-yl)-N-methylmaleimide (100 mg, 0.31 mmol) dissolved in DMF (5 mL), and the whole was stirred for 1.5 hours. The reaction mixture was warmed to room temperature, added with saturated aqueous sodium chloride solution, and extracted with ethyl acetate. The extract was dried over sodium sulfate, and then concentrated under reduced pressure. The residue was purified by column chromatography over silica gel (ethyl acetate:n-hexane=1:2) to obtain 2-bromo-3-(1,5-dimethyl-1H-indol-3-yl)-N-methylmaleimide (100 mg, 95.8%) as red solids.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06589977B1 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-ebb5ce321cad43c6a914920f2a4565a8 |
| 出典メモ | uspto-grants-2003_07 |