関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-[4-(3-Aminophenyl)piperazin-1-yl]ethan-1-one | HCID 11117539 | — |
| 反応物 | Ethyl 2,4-difluoro-5-nitrobenzoate | HCID 22330120 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | Ethyl 4-(3-(4-acetyl-1-piperazinyl)-phenyl)-amino-6-fluoro-3-nitrobenzoate | HCID 86592319 | — |
反応手順
A mixture of ethyl 2,4difluoro-5-nitrobenzoate (22) (1.0 g; 4.33 mmol), 4f (0.95 g; 4.33 mmol) and triethylamine (0.6 ml; 0.33 mmol) in anhydrous NMP (10 ml) was heated to 80° C. for one hour. The cooled mixture was poured into water and extracted with ethyl acetate. The organic extract was dried over magnesium sulphate, concentrated under reduced pressure and purified by column-chromatography on silica gel using ethyl acetate as the eluent. Yield: 1.53 g (82%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06649609B2 |
|---|
| 出典データセット | uspto-grants-2003_11 |
|---|
| ORD ID | ord-f60e53fbf16d4216930254366e7b9374 |
|---|
| 出典メモ | uspto-grants-2003_11 |
|---|
