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Dimethylcarbamoyl Chloride → 5-Methoxy-6-methylpicolinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 反応物 | 3-Methoxy-2-methylpyridine 1-oxide | HCID 12214016 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Methoxy-6-methylpicolinonitrile | HCID 23002417 | 11.8% |
反応手順
To a solution obtained by dissolving 3-methoxy-2-methyl-pyridine-N-oxide (1.57 g, 11.3 mmol) in 30 ml of dichloromethane were added cyanotrimethylsilane (1.12 g, 11.3 mmol) and dimethylcarbamoyl chloride (1.21 g, 11.3 mmol), followed by stirring at room temperature for 9 days. The reaction solution was washed with 10% sodium carbonate aqueous solution and then with water. The organic layer was dried with sodium sulfate and concentrated to remove the solvent, by which 0.198 g (percent yield: 11.8%) of 2-cyano-5-methoxy-6-methylpyridine was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06610853B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-1d1b1b0466054e788516132c7d0acd6c |
| 出典メモ | uspto-grants-2003_08 |