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

HRID 1907364
ノート
印刷プレビュー

反応式

HRID 1907364 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-87fd7a43287d4f67bee9a4e4c8dee556
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08598162B2

反応ノート

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