関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | o-Chlorothiophenol | HCID 80599 | — |
| 反応物 | 1-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine | HCID 4184869 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | Tert-butyl 4-(2-chlorophenylthio)piperidine-1-carboxylate | HCID 58724129 | — |
反応手順
Tert-butyl 4-(methylsulfonyloxy)piperidine-1-carboxylate (2.00 g, 7.16 mmol, prepared according to Blurton et al., WO 00/43362), 2-chlorobenzenethiol (0.898 ml, 7.88 mmol), and potassium carbonate (1.58 g, 11.5 mmol) were stirred together in acetonitrile (15 ml). The reaction was heated to 75° C. and was stirred at that temperature for 15 h. After cooling to room temperature, brine was added, and the mixture was extracted with EtOAc three times. Combined organic layers were dried over MgSO4, filtered and concentrated in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07759339B2 |
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| 出典データセット | uspto-grants-2010_07 |
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| ORD ID | ord-2cc7da808700437b9b7daf0a7c8d0497 |
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| 出典メモ | uspto-grants-2010_07 |
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