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Phenol → 4-(2-Chlorophenylsulfanyl)piperidine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-[(2-Chlorophenyl)thio]-1-[(4-methylphenyl)sulfonyl]piperidine | HCID 13607963 | — |
| 溶媒 | Hydrogen Bromide | HCID 260 | — |
| 生成物 | 4-(2-Chlorophenylsulfanyl)piperidine hydrochloride | HCID 17749802 | — |
反応手順
A mixture of 88.76 g (0.23 mole) of 4-[(2-chlorophenyl)thio]-1-[(4-methylphenyl)sulfonyl]piperidine, 47.0 g (0.50 mole) of phenol and 200 ml of 48% hydrobromic acid was refluxed for 1.5 hr. The reaction mixture was cooled to room temperature and diluted with ice water. The mixture was made alkaline with 50% sodium hydroxide and extracted with diethyl ether. The ether phase was extracted with 1N sulfuric acid. The acidic layer was made alkaline and extracted with methylene chloride. The methylene chloride layer was dried over sodium sulfate, filtered and evaporated to give an oil, the free base of the title compound. The free base was converted to 4.30 g (36.5%) of a white crystalline hydrochloride salt, m.p. 202°-210° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04642348 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-2fd37515aeae47f5b6dce823bd9360b4 |
| 出典メモ | uspto-grants-1987_02 |