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Potassium Carbonate → Ethyl 3-amino-6-nitro-1-benzothiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl Thioglycolate | HCID 12185 | — |
| 反応物 | 2,4-Dinitrobenzonitrile | HCID 554082 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 3-amino-6-nitro-1-benzothiophene-2-carboxylate | HCID 67549245 | 32.4% |
反応手順
2,4-Dinitrobenzonitrile (5.08 g, 26.3 mmol) was dissolved in DMF (55 ml). Potassium carbonate (4.36 g, 31.6 mmol) and ethyl thioglycolate (3.17 g, 26.3 mmol) were added, and the mixture was stirred at room temperature for three days. The reaction solution was concentrated under reduced pressure, diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was recrystallized from ethyl acetate/hexane to obtain 2.27 g of the title compound as crystals (32%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536197B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-9fd42774e03b4419938ca01fdb1efa66 |
| 出典メモ | uspto-grants-2013_09 |