반응식
O.Cl.[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([S:10][CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:6][CH:5]=1.B(O[O-])=[O:18].[Na+]>Cl>[ClH:3].[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([S:10]([CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[O:18])=[CH:8][CH:9]=1참가 물질
4
실험 절차
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. 22°-221° C.
후처리
- customThe reaction mixture was quenched in dilute sodium hydroxide
- extractionthe resulting basic solution was extracted with methylene chloride
- dry with materialThe methylene chloride layer was dried over magnesium sulfate
- customthe solvent was removed in vacuo
- customto give a white solid
출처 및 근거
- ORD 기록
- ord-41df8b20d978420eb4eb3a991d6c8d0b
- 출처 데이터셋
- uspto-grants-1987_02
- 특허 번호
- US04642348
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