化工社化工社 化学情報印刷レポート · 研究参考用
Aniline → alpha-(Phenylamino)benzeneacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Bromo(phenyl)acetic acid | HCID 97919 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | alpha-(Phenylamino)benzeneacetic acid | HCID 19375 | 97% |
反応手順
α-Bromophenylacetic acid (5.01 g, 23.2 mmol.) is dissolved in aniline (25 mL, 274 mmol) and the mixture reacted in a closed vessel under MW irradiation at 120° C. for 5 minutes (LC-MS monitoring: complete conversion). Dichloromethane (DCM) (100 mL) is added to the reaction mixture and the resulting solid is filtered; 2M Na2CO3 (50 mL) is added to the solution, and the aqueous layer is washed with DCM (3×100 mL). The aqueous layer is acidified with 12N HCl (36 mL), and the title compound is recovered as racemic mixture by filtration (5.1 g, 97% yield, white solid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835682B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b9cecdcefa184330a95f0a0c4537d29a |
| 出典メモ | uspto-grants-2014_09 |