関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | Pyrazinecarbonitrile | HCID 73172 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-Chloropyrazine-2-carbonitrile | HCID 292465 | 65.2% |
反応手順
In 90 ml of benzene and 9.2 ml of dimethylformamide there was stirred at room temperature cyanopyrazine (12.7 g; 0.12 M) prepared in Step A above, after which there was added over 10 minutes sulfonyl chloride (64.79 g; 0.48 M). The reaction mixture was stirred for 30 minutes in an ice bath, then allowed to warm up to room temperature gradually, after which it was stirred for 5 hours. The benzene layer was decanted, and the reddish oil residue was extracted three times with ether, after which the combined benzene and ether layers were quenched with ice water and cooled in an ice bath. The combined layers were then neutralized with solid sodium bicarbonate, then separated, and the aqueous layer was extracted with ether. The combined organic layers were washed once with a small amount of water, dried with sodium sulfate, filtered, and the solvent evaporated to give the title compound (11 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04442095 |
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| 出典データセット | uspto-grants-1984_04 |
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| ORD ID | ord-733bffbef1bf4c24911690a97d3791a7 |
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| 出典メモ | uspto-grants-1984_04 |
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