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Water → 4-(4-Benzo[b]thiophen-4-yl-piperazin-1-yl)butan-1-ol

HRID 1907364
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HRID 1907364 반응식
C(=O)([O-])[O-].[K+].[K+].C([O:10][CH2:11][CH2:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][N:18]([C:21]2[C:29]3[CH:28]=[CH:27][S:26][C:25]=3[CH:24]=[CH:23][CH:22]=2)[CH2:17][CH2:16]1)(=O)C.O>CO>[S:26]1[CH:27]=[CH:28][C:29]2[C:21]([N:18]3[CH2:17][CH2:16][N:15]([CH2:14][CH2:13][CH2:12][CH2:11][OH:10])[CH2:20][CH2:19]3)=[CH:22][CH:23]=[CH:24][C:25]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 574825494-(4-Benzo[b]thiophen-4-yl-piperazin-1-yl)butyl acetate

생성물 1

HCID 574825504-(4-Benzo[b]thiophen-4-yl-piperazin-1-yl)butan-1-ol수율 98.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Potassium carbonate (3.87 g, 28 mmol) was added to a solution of 7.76 g (23.3 mmol) of 4-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)butyl acetate in 90% methanol solution (150 ml). The solution mixture was stirred at room temperature for 2 hours. Water was added to the reaction solution, which was then extracted with dichloromethane. The extraction solution was dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (n-hexane:ethyl acetate=2:1→1:1), and concentrated under reduced pressure to obtain 4-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)butan-1-ol (6.65 g) as colorless oil.

후처리

  1. extractionwas then extracted with dichloromethane
  2. dry with materialThe extraction solution was dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by basic silica gel column chromatography (n-hexane:ethyl acetate=2:1→1:1)
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-87fd7a43287d4f67bee9a4e4c8dee556
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598162B2

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