関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Thiopheneacetic acid | HCID 15970 | — |
| 反応物 | N-Hydroxysuccinimide | HCID 80170 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 4-(3-Aminopropylthio)pyridine | HCID 15227695 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[3-(2-Thienylacetylamino)propylthio]pyridine | HCID 15231493 | 86.3% |
反応手順
To a solution of 913 mg (6.42 mmol) of 2-thienylacetic acid and 961 mg (8.35 mmol) of N-hydroxysuccinimide in 65 ml of methylene chloride, 1.48 g (7.70 mmol) of 1-ethyl-3 (3-dimethylaminopropyl)carbodiimide hydrochloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 1 hour. Further, 1.08 g (6.42 mmol) of 4-(3-aminopropylthio)pyridine was added, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was washed with water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10) to obtain powder. The powder thus obtained was washed with ether and dried to obtain 1.62 g of the desired compound Lyield: 86.3%, pale yellow powder).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05246948 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-1e860fd9a7364d6a91a5b65f8afc24f0 |
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| 出典メモ | uspto-grants-1993_09 |
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