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4-Cyanopyridine → Pyridine-4-amidine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Cyanopyridine | HCID 7506 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Pyridine-4-amidine hydrochloride | HCID 2776844 | 47.3% |
反応手順
Sodium methoxide (0.54 g) and 4-cyanopyridine (10.4 g) were combined in anhydrous methanol (100 ml) and stirred at room temperature for 18 h, under a nitrogen atmosphere. Ammonium chloride (5.99 g) was then added, and the mixture heated to reflux for 4 h, under a calcium chloride guard tube. The reaction was cooled, evaporated under reduced pressure, re-suspended in ethanol (120 ml) and heated to reflux for another 15 min. The resultant white precipitate was filtered off, dried, then triturated with ice-cold water and dried under vacuum at 40° C. to yield the title compound as a white solid (7.44 g, 47%). Two further crops were obtained through concentration of the ethanol filtrate (total yield 12.1 g, 77%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06809100B2 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-0e21b225ba294f82a2884000b6fecbce |
| 出典メモ | uspto-grants-2004_10 |