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

HRID 605783
ノート
印刷プレビュー

反応式

HRID 605783 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 57507753HCID 57507753、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c92d113891444e3aa247253693266e20
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915261B2

反応ノート

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