関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| 反応物 | Ethyl 2-amino-1-benzothiophene-3-carboxylate | HCID 699464 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Ethyl 2-(5-fluoro-2-nitroanilino)benzo[b]thiophene-3-carboxylate | HCID 18422317 | 44.9% |
反応手順
Ethyl 2-aminobenzo[b]thiophene-3-carboxylate (69.3 g) and 2,4-difluoronitrobenzene (50 g) were dissolved in dimethyl sulfoxide (550 ml) and heated to 50° C. Thereto was added potassium carbonate (63 g) and the mixture was stirred at 100° C. for 70 min. After cooling, the reaction mixture was allowed to cool to 70° C. and poured into water (2.5 L). The reaction mixture was allowed to stand still, and filtered. The filtrated orange crystals were washed with ethyl acetate to give ethyl 2-(5-fluoro-2-nitroanilino)benzo[b]thiophene-3-carboxylate (50.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06271225B1 |
|---|
| 出典データセット | uspto-grants-2001_08 |
|---|
| ORD ID | ord-81c6691c52ce497596d581f65bc3fe64 |
|---|
| 出典メモ | uspto-grants-2001_08 |
|---|