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Hydrochloric Acid → (E)-2-(2-Fluorostyryl)-1-(2-pyridyl)-1H-benzimidazole hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N1-(pyridin-2-yl)benzene-1,2-diamine | HCID 752150 | — |
| 反応物 | (2E)-3-(2-Fluorophenyl)acryloyl chloride | HCID 5706469 | — |
| 反応物 | (E)-1-(2-pyridyl)-2-styryl-1H-benzimidazole | HCID 9796241 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (E)-2-(2-Fluorostyryl)-1-(2-pyridyl)-1H-benzimidazole hydrochloride | HCID 9906470 | — |
反応手順
Free base of the titled compound was prepared from N-(2-pyridyl)-o-phenylenediamine and (E)-2-fluorocinnamoyl chloride (Amino, Y.; Kawada, K.; Toi, K.; Kumashiro, I.; Fukushima, K. Chem. Pharm. Bull, 1988, 36, 4426) according to the preparation of (E)-1-(2-pyridyl)-2-styryl-1H-benzimidazole (Example 1, method A). The free base was dissolved with a 10% methanol solution of hydrogen chloride (5 ml). Concentration and recrystallization from ethyl acetate/ethanol yielded the titled compound. MW: 351.81; mp: 226.0-228.0° C.; 1H-NMR (DMSO) δ: 8.92-8.87 (1H, m), 8.39-8.29 (1H, m), 8.29 (1H, d, J=16.1 Hz), 7.99-7.79 (4H, m), 7.70-7.51 (4H, m), 7.44-7.31 (3H, 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-d129c2b05840490f94a91469e471a5fd |
| 出典メモ | uspto-grants-2004_03 |