関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,5-Difluoroaniline | HCID 67775 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Ethyl bromophenylacetate | HCID 97780 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl 2-(2,5-difluorophenylamino)-2-phenylacetate | HCID 58556973 | 67% |
反応手順
2,5-Difluoroaniline (0.19 mL, 1.85 mmol), ethyl 2-bromo-2-phenylacetate (0.22 mL, 1.23 mmol), and DIPEA (0.32 mL, 1.85 mmol) are dissolved in acetonitrile (3 mL) and heated under MW irradiation at 100° C. for 6 hours and then at 110° C. for 4 hours. Acetonitrile is evaporated and the crude is purified by flash chromatography (Petroleum ether/EtOAc=97/3) to obtain intermediate I104 as a white solid (240 mg, 67% yield).
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-7adf7ece2fe84b79a4fb7b0fe2f787f8 |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
