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Triethylamine → HCID 178520201、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloro-1-methylpyridinium iodide | HCID 167069 | — |
| 反応物 | 2-(3-Fluoroquinolin-8-yl)acetic acid hydrogen chloride | HCID 68755992 | — |
| 反応物 | HCID 178509325 | HCID 178509325 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178520201 | HCID 178520201 | — |
反応手順
4-Bromo-3-(4H-1,2,4-triazol-3-yl)thiophen-2-amine (17 mg, 69.4 umol), 2-(3-fluoroquinolin-8-yl)acetic acid hydrogen chloride (22 mg, 91.0 umol), 2-chloro-1-methylpyridinium iodide (101 mg, 395 umol) and triethylamine (0.2 ml) in methylene chloride (1 ml) was heated to reflux. After stirring for 1 h, the solution was concentrated and the residue was purified by HPLC to yield N-(4-bromo-3-(1H-1,2,4-triazol-3-yl)thiophen-2-yl)-2-(3-fluoroquinolin-8-yl)acetamide. Method [7] retention time 5.67 min by HPLC (M+ 432 and 434) and (M+Na 454 and 456). 1H NMR (300 MHz, CDCl3) δ 12.25 (s, 1H), 8.83 (d, J=3.3 Hz, 1H), 7.87 (m, 2H), 7.80 (d, J=6.0 Hz, 1H), 7.73 (s, 1H), 7.66 (t, J=7.8 Hz, 1H), 6.90 (s, 1H), 6.70 (broad s, 2H), 4.56 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09073891B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-953f87d9a1194207bd118839ffecdf0f |
| 出典メモ | uspto-grants-2015_07 |