化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → Propanenitrile, 2-methyl-2-(methylsulfonyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (Methylsulfonyl)acetonitrile | HCID 75283 | — |
| 生成物 | Propanenitrile, 2-methyl-2-(methylsulfonyl)- | HCID 3014848 | 78% |
反応手順
To a solution of 2-(methylsulfonyl)acetonitrile (60 g, 504 mmol) in DMF (252 mL) at 0° C. was added potassium carbonate (209 g, 1511 mmol) portion-wise, followed by iodomethane (136 mL, 1511 mmol). After 15 minutes, the ice bath was removed and the reaction was stirred at RT for 48 hours. The reaction mixture was filtered through a Celite pad, and the filter cake was rinsed with ethyl acetate and ether. The combined filtrates were concentrated and partitioned between ether and water. The organic portion was dried over sodium sulfate, filtered, and concentrated in vacuo to afford the titled intermediate (58 g, 78% yield) as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09309263B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-2e10f9ea604e493a8d783fc1f5d52e00 |
| 出典メモ | uspto-grants-2016_04 |