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Triethylamine → 3-[3-(Thenoylamino)propylthio]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Thiophenecarbonyl chloride | HCID 78928 | — |
| 反応物 | 3-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079113 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-[3-(Thenoylamino)propylthio]pyridine | HCID 19079144 | 85.4% |
反応手順
To a solution of 2.00 g (8.29 mmol) of 3-(3-aminopropylthio)pyridine dihydrochloride and 4.16 ml (29.9 mmol) of triethylamine in 80 ml of methylene chloride, 1.06 ml (9.95 mmol) of 2-thenoyl chloride was added under ice-cooling with stirring. The-mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain powder. The powder was washed with ether and dried to obtain 1.97 g of the desired compound (yield: 85.3%, yellow powder). mp: 66.0°-67.0° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05767121 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-5bb4d65ac01e4d0995222c13064b0ce9 |
| 出典メモ | uspto-grants-1998_06 |