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Sodium Perborate → 4-[(4-Chlorophenyl)sulfinyl]piperidine, Monohydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Perborate | HCID 517072 | — |
| 反応物 | 4-[(p-Chlorophenyl)thio]piperidine hydrochloride hydrate | HCID 20217779 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 4-[(4-Chlorophenyl)sulfinyl]piperidine, Monohydrochloride | HCID 85527719 | — |
反応手順
A solution of 5.78 g (0.020 mole) of 4-[(p-chlorophenyl)thio]piperidine hydrochloride hydrate and 4.61 g (0.030 mole) of sodium perborate in 200 ml of dilute hydrochloride acid was stirred at room temperature overnight. The reaction mixture was quenched in dilute sodium hydroxide and the resulting basic solution was extracted with methylene chloride. The methylene chloride layer was dried over magnesium sulfate and the solvent was removed in vacuo to give a white solid, the free base of the title compound. The free base was reacted with ethereal hydrogen chloride and the salt was recrystallized from methanol-diethyl ether to give the product as a white crystalline solid, m.p. 220°-221° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04593102 |
| 出典データセット | uspto-grants-1986_06 |
| ORD ID | ord-40b4ee8967784a629c1fcd66eb52f83e |
| 出典メモ | uspto-grants-1986_06 |