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Iodine → 4-[4-[4-Hydroxy-4-[4-(4-methoxybutoxy)phenyl]piperidin-1-yl]phenyl]piperazine-1-carboxylic acid benzyl ester

HRID 1816771
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HRID 1816771 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH3:14])=[CH:4][CH:3]=1.[Mg].II.IC(I)C.[CH2:22]([O:29][C:30]([N:32]1[CH2:37][CH2:36][N:35]([C:38]2[CH:43]=[CH:42][C:41]([N:44]3[CH2:49][CH2:48][C:47](=[O:50])[CH2:46][CH2:45]3)=[CH:40][CH:39]=2)[CH2:34][CH2:33]1)=[O:31])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[Cl-].[NH4+]>O1CCCC1.C(OCC)(=O)C>[CH2:22]([O:29][C:30]([N:32]1[CH2:37][CH2:36][N:35]([C:38]2[CH:43]=[CH:42][C:41]([N:44]3[CH2:49][CH2:48][C:47]([OH:50])([C:2]4[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH3:14])=[CH:4][CH:3]=4)[CH2:46][CH2:45]3)=[CH:40][CH:39]=2)[CH2:34][CH2:33]1)=[O:31])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1
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참가 물질

9

반응물 6

HCID 807IodineHCID 25517Ammonium ChlorideHCID 68980DiiodoethaneHCID 5462224MagnesiumHCID 224947841-Bromo-4-(4-methoxybutoxy)benzeneHCID 543714504-[4-(4-Oxopiperidin-1-yl)phenyl]piperazine-1-carboxylic acid benzyl ester

생성물 1

HCID 54570705
4-[4-[4-Hydroxy-4-[4-(4-methoxybutoxy)phenyl]piperidin-1-yl]phenyl]piperazine-1-carboxylic acid benzyl ester
수율 47.5%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To the solution of 1-bromo-4-(4-methoxybutoxy)benzene (4.94 g) and magnesium (463 mg) in tetrahydrofuran (50 ml) was added iodine at room temperature. The solution was refluxed for 7.5 hours, during which period diiodoethane was added to the mixture. After cooling to 0° C., 4-[4-(4-oxopiperidin-1-yl)phenyl]piperazine-1-carboxylic acid benzyl ester (4.94 g) in tetrahydrofuran (20 ml) was added dropwise with stirring to the solution. The mixture was stirred at room temperature for 2 hours. The reaction mixture was added to a mixture of ammonium chloride solution and ethyl acetate. The organic layer was taken, washed with brine, sodium hydrogen carbonate solution and brine and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (50:1 dichloromethane-methanol elution) to give 4-[4-[4-hydroxy-4-[4-(4-methoxybutoxy)phenyl]piperidin-1-yl]phenyl]piperazine-1-carboxylic acid benzyl ester (3.42 g).

후처리

  1. additionwas added to the mixture
  2. stirringThe mixture was stirred at room temperature for 2 hours
  3. washwashed with brine, sodium hydrogen carbonate solution and brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe magnesium sulfate was filtered off
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (50:1 dichloromethane-methanol elution)

출처 및 근거

ORD 기록
ord-1661f82eb00646bbbbdf9e7af5e256f2
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06884868B1

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