化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → N-(2-Fluoro-1,1-dimethylethyl)-2,4-difluorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,4-Difluorobenzoic acid | HCID 74102 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-Fluoro-2-methylpropan-2-amine hydrochloride | HCID 13935251 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-Fluoro-1,1-dimethylethyl)-2,4-difluorobenzamide | HCID 10198515 | 44% |
反応手順
WSC HCl (1.15 g, 6 mmol) was added to a mixture of 2,4-difluorobenzoic acid (0.95 g, 6 mmol), 2-fluoro-1,1-dimethylethylamine hydrochloride (J. Med. Chem., 34, 29-37(1991): 0.77 g, 6 mmol), HOBt (0.81 g, 6 mmol) and triethylamine (0.91 g, 9 mmol) in methylene chloride (15 ml), and stirred at room temperature for 3 hours. The reaction mixture was concentrated, diluted with ethyl acetate and washed with saturated aqueous NaHCO3, 1N hydrochloric acid, saturated aqueous NaHCO3 and brine, successively, dried over MgSO4 and concentrated under a reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=20/1) to give the title compound (0.61 g; 44%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06384033B1 |
| 出典データセット | uspto-grants-2002_05 |
| ORD ID | ord-3b416deca68a470ea52778d915c619fb |
| 出典メモ | uspto-grants-2002_05 |