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Oxalic Acid → (E)-1-(2-Pyridyl)-2-[2-(4-pyridyl)ethenyl]-1H-benzimidazole oxalate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | 4-Pyridinecarboxaldehyde | HCID 13389 | — |
| 反応物 | 2-Methyl-1-(pyridin-2-yl)-1H-benzimidazole | HCID 22736643 | — |
| 反応物 | (E)-1-(2-Pyridyl)-2-[2-(2-pyridyl)ethenyl]-1H-benzimidazole dihydrochloride | HCID 22736657 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (E)-1-(2-Pyridyl)-2-[2-(4-pyridyl)ethenyl]-1H-benzimidazole oxalate | HCID 22736688 | — |
反応手順
Free base of the titled compound was prepared from 2-methyl-1-(2-pyridyl)-1H-benzimidazole and pyridine4-carboxaldehyde according to the preparation of (E)-1-(2-pyridyl)-2-[2-(2-pyridyl)ethenyl]-1H-benzimidazole dihydrochloride Example 44). The free base and oxalic acid were dissolved into MeOH. Concentration and recrystalization from ethyl MeOH/Et2O/n-hexane yielded the titled compound. MW: 388.39; mp: 203.6-205.3° C. (decomposed); 1H-NMR (DMSO) δ: 8.81-8.75 (1H, m), 8.62-8.55 (2H, m), 8.20 (1H, dt, J=1.9,7.7 Hz), 7.88 (1H, d, J=16.0 Hz), 7.81-7.74 (2H, m), 7.69-7.60 (3H, m), 7.52-7.46 (1H, m), 7.47 (1H, d, J=16.0 Hz) 7.40-7.28 (2H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713482B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-e3440b1ca2a5458fa63bdfa72706bbc7 |
| 出典メモ | uspto-grants-2004_03 |