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Oxalic Acid → (E)-1-(2-Pyridyl)-2-[2-(3-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 | 3-Pyridinecarboxaldehyde | HCID 10371 | — |
| 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-(3-pyridyl)ethenyl]-1H-benzimidazole oxalate | HCID 22736735 | — |
反応手順
Free base of the titled compound was prepared from 2-methyl-1-(2-pyridyl)-1H-benzimidazole and pyridine-3-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 recrystallization from ethyl MeOH/EtOH yielded the titled compound. MW: 388.39; mp: 193.3-194.1° C. (decomposed); 1H-NMR (DMSO) δ: 8.86-8.81 (1H, m), 8.80-8.76 (1H, m), 8.53 (1H, dd, J=4.8, 1.5 Hz), 8.19 (1H, dt, J=7.8, 1.9 Hz), 8.12-8.05 (1H, m), 7.93 (1H, d, J=16.0 Hz), 7.76 (2H, d, J=7.9 Hz), 7.68-7.61 (1H, m), 7.51-7.25 (4H, m), 7.33 (1H, d, J=16.0 Hz).
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-470c5c747c114e969224ae787b24df53 |
| 出典メモ | uspto-grants-2004_03 |