化工社化工社 化学情報印刷レポート · 研究参考用
Tert-Butylamine → N-t-Butyl-4-chloro-2-fluorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 4-Chloro-2-fluorobenzoic acid | HCID 99152 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-t-Butyl-4-chloro-2-fluorobenzamide | HCID 10130797 | 96% |
反応手順
To a suspension of 4-chloro-2-fluorobenzoic acid (0.3494 g, 2.00 mmol) in methylene chloride (10 ml) were added t-butylamine (0.32 ml, 3.05 mmol) and HOBt (0.3248 g, 2.40 mmol), and then WSC HCl (0.4596 g, 2.40 mmol) was added and stirred for 3 hours. The reaction mixture was added into water and extracted three times with ethyl acetate. The combined extracts were dried over MgSO4. The solvent was evaporated and the residue was purified by silica gel chromatography (hexane/ethyl acetate=5/1) to give the title compound (0.4403 g; 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06936736B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-15e4102d01554bf98427b75ddeba1303 |
| 出典メモ | uspto-grants-2005_08 |