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Ethyl 3-aminobenzoate → Ethyl 3-[(2-acetylthiomethyl-3-phenylpropionyl)amino]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 3-aminobenzoate | HCID 11400 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 2-[(Acetylthio)methyl]-3-phenylpropionic Acid | HCID 9991796 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 3-[(2-acetylthiomethyl-3-phenylpropionyl)amino]benzoate | HCID 15670143 | 67.5% |
反応手順
2-Acetylthiomethyl-3-phenylpropionic acid (11.9 g) and ethyl 3-aminobenzoate (8.26 g) are dissolved in dichloromethane (150 ml), and thereto are added 4-dimethylaminopyridine (0.61 g) and EDC.HCl (10.54 g), and the mixture is stirred at room temperature overnight. The reaction mixture is washed with saturated aqueous citric acid solution, saturated aqueous sodium chloride solution and saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution in this order, dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. The residue is washed with diethyl ether to give the title compound (13 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05210266 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-0523243cb0aa491d8a790635ab59cd54 |
| 出典メモ | uspto-grants-1993_05 |