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Oxalic Acid → (E)-1-(2-Pyridyl)-2-styryl-5-methoxy-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-Methoxy-2-nitroaniline | HCID 66793 | — |
| 反応物 | (E)-1-(2-pyridyl)-2-styryl-5-trifluoromethyl-1H-benzimidazole | HCID 22736704 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (E)-1-(2-Pyridyl)-2-styryl-5-methoxy-1H-benzimidazole oxalate | HCID 22736663 | — |
反応手順
Free base of the titled compound was prepared from 4-methoxy-2-nitroaniline according to the preparation of (E)-1-(2-pyridyl)-2-styryl-5-trifluoromethyl-1H-benzimidazole (Example 57). The free base and oxalic acid were dissolved into ethyl acetate. Concentration and recrystallization from ethyl acetate/n-hexane yielded the titled compound. MW: 417.42; mp: 187.0-188.0° C.; 1H-NMR (DMSO-d6) δ: 8.76 (1H, dd, J=5.0, 1.3 Hz), 8.17 (1H, td, J=7.8,2.0 Hz), 7.85 (1H, d, J=15.8 Hz), 7.72 (1H, d, J=8.1 Hz), 7.65-7.58 (3H, m), 7.42-7.30 (4H, m), 7.26 (1H, d, J=2.2 Hz), 7.17 (1H, d, J=16.1 Hz), 6.90 (1H, dd, J=8.8, 2.6 Hz), 3.83 (3H, s).
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-3ad2815c978041cfa15e99b2223ef6cd |
| 出典メモ | uspto-grants-2004_03 |