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Dimethylcarbamoyl Chloride → 4-Phenyl-2-pyridinecarbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 反応物 | 4-Phenylpyridine-1-oxide | HCID 70803 | — |
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 溶媒 | Nitroethane | HCID 6587 | — |
| 生成物 | 4-Phenyl-2-pyridinecarbonitrile | HCID 87758 | 89% |
反応手順
4-Phenylpyridine N-oxide (3.13 g, 18.3 mmol) was dissolved in nitroethane (30 ml), and trimethylsilyl cyanide (2.0 g, 20.2 mmol) and N,N-dimethylcarbamoyl chloride (1.7 ml, 18.5 mmol) were added thereto. The reaction mixture was stirred at room temperature for 45 hrs, concentrated under reduced pressure, combined with saturated aqueous sodium hydrogen carbonate solution and extracted with ethyl acetate. The extract was washed with saturated brine and dried. The solvent was evaporated under reduced pressure. The obtained crystals were collected by filtration, washed with diisopropyl ether and dried to give the titled compound (2.87 g, 89%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07767665B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-aafbc8291af34cd19099661c64b04630 |
| 出典メモ | uspto-grants-2010_08 |