関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloropropionyl chloride | HCID 111019 | — |
| 反応物 | Methyl 4-aminothiophene-3-carboxylate | HCID 2777610 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Rac-4-(2-chloro-propionylamino)-thiophene-3-carboxylic acid methyl ester | HCID 68688356 | 82% |
反応手順
To a suspension of 4-amino-thiophene-3-carboxylic acid methyl ester (2.0g) in dichloromethane (25 mL) was added 2-chloropropionyl chloride (1.13 mL). The reaction mixture was then cooled down to −15° C. and a solution of triethylamine (3.2 mL) in dichloromethane (5 mL) was slowly added over 30 minutes. After such time the reaction mixture was allowed to warm up to room temperature, and the solution was washed twice with water, dried over sodium sulfate and then concentrated in vacuo. The residue was purified by column chromatography to yield the title compound as a light yellow solid (2.1g, 82%). MS (EI): 247.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07732452B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-b604834c7358483795593421fbc68b98 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|