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Sodium Hydroxide → 3-(4-Phthalimidobutylthio)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-(4-Bromobutyl)phthalimide | HCID 93575 | — |
| 反応物 | 3-Dimethylaminocarbamoylthiopyridine | HCID 19079082 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(4-Phthalimidobutylthio)pyridine | HCID 19079103 | 4.5% |
反応手順
To a solution of 3.64 g (20 mmol) of 3-dimethylaminocarbamoylthiopyridine in 100 ml of methanol was added 1.6 g (40 mmol) of sodium hydroxide. The mixture was heated and refluxed for 3 hours under nitrogen atmosphere. After cooling, 5.64 g (20 mmol) of N-(4-bromobutyl)phthalimide was added. The mixture was heated and refluxed for 2.5 hours. The solvent was distilled off and chloroform was added to the residue. The mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane=1:1) to obtain 280 mg of the desired compound (4.5%, colorless oil).
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-e94fd6bfa01d4f6e8f7a35095695cdbe |
| 出典メモ | uspto-grants-1993_09 |