化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → Methyl 4-{2-[(benzofuran-2-yl-carbonyl)amino]ethylsulfanyl}benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzofuran-2-carboxylic acid | HCID 10331 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 反応物 | Methyl 4-(2-aminoethylsulfanyl)benzoate hydrochloride | HCID 66687893 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-{2-[(benzofuran-2-yl-carbonyl)amino]ethylsulfanyl}benzoate | HCID 66687946 | 38.8% |
反応手順
Methyl 4-(2-aminoethylsulfanyl)benzoate hydrochloride (0.248 g, 1.00 mmol), was combined with benzofuran-2-carboxylic acid (0.162 g, 1.00 mmol) and HBTU (0.379 g, 1.00 mmol) in DMF (5 ml) at room temperature. Triethylamine (0.307 ml, 2.2 mmol) was added and the reaction mixture was stirred at room temperature overnight. Saturated aqueous NaHCO3 (15 ml) was added to give precipitates which was broken up by the addition of water (20 ml). The solid was filtered and the cake was dissolved in ethyl acetate. The residual water was removed by pipette and hexane was added to give methyl 4-{2-[(benzofuran-2-yl-carbonyl)-amino]ethylsulfanyl}benzoate (0.138 g) as a gum which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07420089B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-14f61712884949cfaf2783c6c5b1ae07 |
| 出典メモ | uspto-grants-2008_09 |