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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 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Phenylpyridine-1-oxide | HCID 70803 | — |
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Phenyl-2-pyridinecarbonitrile | HCID 87758 | — |
反応手順
To a stirred solution of 4-phenylpyridine N-oxide (25 g, 0.146 mmol) in dichloromethane (200 ml) at room temperature was added trimethylsilyl cyanide (17.4 g), followed by the slow addition of dimethyl carbamyl chloride (16.2 ml) in dichloromethane (50 ml) over a 30 minute period. The reaction mixture was stirred at room temperature for one day, and then to it potassium carbonate solution (10%,150 ml) was added slowly. Stirring continued for an additional 30 minutes, the organic layer was separated, and the aqueous layer was extracted with dichloromethane. The extracts were combined and dried over magnesium sulfate. Evaporation in vacuo gave a crude reaction product (35 g) as a white solid. It was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05494919 |
| 出典データセット | uspto-grants-1996_02 |
| ORD ID | ord-f04bcee204ef4760aef8b2232e22f265 |
| 出典メモ | uspto-grants-1996_02 |