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Hydrogen chloride-ethyl acetate → 4-({4-[(3-Fluorobenzyl)oxy]phenyl}sulfanyl)piperidine

HRID 2074231
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반응식

HRID 2074231 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][CH:29]=1)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][CH:14]2[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH2:15]2)=[CH:9][CH:8]=1.Cl.CCOC(C)=O>CCOC(C)=O>[F:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][CH:29]=1)[CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10]([S:13][CH:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)=[CH:11][CH:12]=1
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참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 57507753HCID 57507753, 화합물

생성물 1

HCID 574217934-({4-[(3-Fluorobenzyl)oxy]phenyl}sulfanyl)piperidine수율 86.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Tert-butyl 4-({4-[(3-fluorobenzyl)oxy]phenyl}sulfanyl)piperidine-1-carboxylate (501 mg) was dissolved in EtOAc (5 ml), and a 4 M hydrogen chloride/EtOAc solution (3 ml) was added thereto, followed by stirring at room temperature for 3 hours. Then, the solvent was evaporated under reduced pressure. The residue was dissolved in water, neutralized with an aqueous 1 M sodium hydroxide solution, followed by extraction with chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain 4-({4-[(3-fluorobenzyl)oxy]phenyl}sulfanyl)piperidine (328 mg).

후처리

  1. customThen, the solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in water
  3. extractionfollowed by extraction with chloroform
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-ed5179b1068840c48684d8fbea78f00f
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919494B2

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