Sodium Perborate → 4-[(4-Chlorophenyl)sulfinyl]piperidine, Monohydrochloride

HRID 1981794

반응식

HRID 1981794 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]=1

참가 물질

4

반응물 2

HCID 517072Sodium PerborateHCID 202177794-[(p-Chlorophenyl)thio]piperidine hydrochloride hydrate

생성물 1

HCID 855277194-[(4-Chlorophenyl)sulfinyl]piperidine, Monohydrochloride

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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. 220°-221° C.

후처리

  1. customThe reaction mixture was quenched in dilute sodium hydroxide
  2. extractionthe resulting basic solution was extracted with methylene chloride
  3. dry with materialThe methylene chloride layer was dried over magnesium sulfate
  4. customthe solvent was removed in vacuo
  5. customto give a white solid

출처 및 근거

ORD 기록
ord-40b4ee8967784a629c1fcd66eb52f83e
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04593102

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