関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloropyridine-2-carbonitrile | HCID 118424 | — |
| 反応物 | HCID 178480602 | HCID 178480602 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Cyano-6-(1-methyl-1H-imidazol-2-yl)thiopyridine | HCID 22939455 | 263.6% |
反応手順
2-Mercapto-1-methyl-1H-imidazole (0.91 g, 7.94 mmol) and sodium hydride (60% in oil, 0.35 g, 8.66 mmol) were dissolved in DMF (30 ml), and 2-chloro-6-cyanopyridine (1.05 g, 3.00 mmol) was added thereto. The reaction mixture was stirred at 70° C. for 18 hrs and 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 (1.71 g, ca. 100%) as pale yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07399759B2 |
|---|
| 出典データセット | uspto-grants-2008_07 |
|---|
| ORD ID | ord-99b20cab5ce8403285552e0902eba362 |
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| 出典メモ | uspto-grants-2008_07 |
|---|
