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Sodium Hydroxide → 4-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol

HRID 269899
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HRID 269899 반응식
Cl.[CH:2]1([CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]3[CH:22]=[CH:21][C:20]([OH:23])=[C:19]([F:24])[CH:18]=3)[CH2:13][CH2:12]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.C(=O)([O-])O.[Na+].[OH-].[Na+]>C(OCC)(=O)C>[CH:2]1([CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]3[CH:22]=[CH:21][C:20]([OH:23])=[C:19]([F:24])[CH:18]=3)[CH2:13][CH2:12]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 231114144-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol hydrochloride

생성물 1

HCID 231114094-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol수율 69.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

4-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol hydrochloride (1.45 g) was suspended in ethyl acetate, and to which saturated aqueous sodium hydrogencarbonate solution and 2 grains of sodium hydroxide were added by the order stated, to effect distribution. The ethyl acetate layer was washed with saturated saline solution, dried over anhydrous magnesium sulfate, and the solvent was distilled off. Purifying the resulting crude product on silica gel column chromatography (eluent, chloroform: methanol=10:1), 4-[4-(3-cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol (910 mg) was obtained.

후처리

  1. washThe ethyl acetate layer was washed with saturated saline solution
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off
  4. customPurifying the resulting crude product on silica gel column chromatography (eluent, chloroform: methanol=10:1)

출처 및 근거

ORD 기록
ord-853df0823b0b46e4a000ae41f5b8f83d
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07449466B2

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