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Triethylamine → 4-[3-(3,5-Dimethoxybenzoylamino)propylthio]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,5-Dimethoxybenzoyl chloride | HCID 87003 | — |
| 反応物 | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[3-(3,5-Dimethoxybenzoylamino)propylthio]pyridine | HCID 15231488 | 87.7% |
反応手順
To a solution of 1.00 g (4.15 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 2.77 ml (19.8 mmol) of triethylamine in 40 ml of methylene chloride was added 995 mg (4.96 mmol) of 3,5-dimethoxybenzoyl 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: ethyl acetate) to obtain 1.21 g of the desired compound (87.7%, pale yellow powder), mp: 110.0°-111.0° 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-eaa03d3d21724503ab66e842fd29b46d |
| 出典メモ | uspto-grants-1993_09 |