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Triethylamine → 4-(3-(cinnamoylamino)propylthio]pyridine Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Phenylprop-2-enoyl chloride | HCID 66023 | — |
| 反応物 | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(3-(cinnamoylamino)propylthio]pyridine Hydrochloride | HCID 67653231 | 88.8% |
反応手順
To a solution of 1.00 g (4.15 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 2.78 ml (19.9 mmol) of triethylamine in 40 ml of methylene chloride was added 830 mg (4.98 mmol) of cinnamoyl chloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10) to obtain the powder which was washed with ether and dried to obtain 1.10 g of the desired compound (free base) (88.8%, colorless powder), mp: 116.0°-11.7° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246948 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-f15dd3fd1fd04d268953342d248889ee |
| 出典メモ | uspto-grants-1993_09 |