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Tetrahydrofuran → 2-Cyano-6-[2-(dimethylamino)ethylthio]pyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Captamine Hydrochloride | HCID 25798 | — |
| 反応物 | 6-Chloropyrazine-2-carbonitrile | HCID 81303 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Cyano-6-[2-(dimethylamino)ethylthio]pyrazine | HCID 22939535 | 48% |
反応手順
2-Dimethylaminoethanethiol hydrochloride salt (1.46 g, 10.0 mmol) and sodium hydride (60% in oil, 0.88 g, 22.0 mmol) were added to THF (50 ml), and 2-chloro-6-cyanopyrazine (1.40 g, 10.0 mmol) was added thereto. The mixture was stirred at room temperature for 18 hrs. The reaction mixture was combined with ethyl acetate and water. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was recrystallized from n-hexane-ethyl acetate to give the titled compound (1.00 g, 48%) as pale yellow crystals.
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-d2ceec83bc854dd18583a6682f2a90d1 |
| 出典メモ | uspto-grants-2010_08 |