関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Hexafluorobenzene | HCID 9805 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Phenylpiperidin-4-ol | HCID 96387 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(2,3,4,5,6-Pentafluorophenoxy)-4-phenylpiperidine | HCID 14649978 | 44% |
反応手順
A suspension of sodium hydride (60% in oil, 6.4 g) in 50 ml of dry dimethylformamide was treated with a solution of 2.5 g of 4-hydroxy-4-phenylpiperidine in 100 ml of dry dimethylformamide over a period of ten minutes. After heating at 50° C. for 30 minutes the mixture was cooled to 5° C. and a solution of 18.6 ml of hexafluorobenzene in 100 ml of dry dimethylformamide was added, dropwise, over a period of 30 minutes. The reaction mixture was then stirred at ambient temperature for 20 hours, poured into 500 ml of water, and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered, and concentrated to yield 21 g (44%) of 4-(2,3,4,5,6-pentafluorophenoxy)-4-phenylpiperidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04853384 |
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| 出典データセット | uspto-grants-1989_08 |
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| ORD ID | ord-e9956c2bbc664c2f82cb3e49806803ce |
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| 出典メモ | uspto-grants-1989_08 |
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