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Sodium hydride → 4-(2-(4-Fluorophenylthio)eth-1-yl)-1-tert-butoxycarbonylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Fluorothiophenol | HCID 67789 | — |
| 反応物 | Tert-butyl 4-(2-iodoethyl)piperidine-1-carboxylate | HCID 9974426 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(2-(4-Fluorophenylthio)eth-1-yl)-1-tert-butoxycarbonylpiperidine | HCID 18187481 | 95.2% |
反応手順
To a slurry of sodium hydride (47 mg, 60% in mineral oil, 1.2 mmol) in tetrahydrofuran at 0° C. was added 4-fluorothiophenol (0.1 mL, 0.94 mmol). The reaction mixture was warmed to r.t. for 20 min, followed by addition of 4-(2-iodo-1-ethyl)-1-tert-butoxycarbonyl-piperidine (265 mg, 0.78 mmol, from Step C). The reaction was then heated to reflux for 10 min, cooled and diluted with ether. The organic layer was washed with 1 N NaOH, dried over MgSO4 and concentrated to provide 252 mg (95%) of the title compound. ESI-MS: 340.0 (M+H); HPLC A: 4.07 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06498161B1 |
| 出典データセット | uspto-grants-2002_12 |
| ORD ID | ord-db5a740d5315411b98cb0561110f776b |
| 出典メモ | uspto-grants-2002_12 |