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Piperazine → 2-(4-Bromophenyl)-2-isopropyl-5-(4-phenylpiperazine-1-yl)pentanoic acid methyl ester

HRID 547984
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반응식

HRID 547984 반응식
[CH3:1][O:2][C:3](=[O:19])[C:4]([C:12]1[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][CH:13]=1)([CH:9]([CH3:11])[CH3:10])[CH2:5][CH2:6][CH2:7]Br.[C:20]1([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.N1CCNCC1.CCN(CC)CC.I([O-])(=O)=O.[Na+]>C(#N)C>[CH3:1][O:2][C:3](=[O:19])[C:4]([C:12]1[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][CH:13]=1)([CH:9]([CH3:11])[CH3:10])[CH2:5][CH2:6][CH2:7][N:29]1[CH2:30][CH2:31][N:26]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:27][CH2:28]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 4837PiperazineHCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 23675764Sodium IodateHCID 468558605-Bromo-2-(4-bromophenyl)-2-isopropylpentanoic acid methyl ester

생성물 1

HCID 461867402-(4-Bromophenyl)-2-isopropyl-5-(4-phenylpiperazine-1-yl)pentanoic acid methyl ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

After the 5-bromo-2-(4-bromophenyl)-2-isopropylpentanoic acid methyl ester (200 mg, 1 eq) was dissolved in acetonitrile, 4-phenylpiperazine (70 mg, 1 eq) as a piperazine derivative, Et3N (0.06 ml, 1.2 eq), and sodium iodate were added into the solution and heated and refluxed for 3 hours. When the reaction was completed, the precipitate was filtrated and the mixture was vacuum distilled and extracted with ethyl acetate and water. After the organic layer was washed with 1N HCl and saturated NaHCO3, the target compound 2-(4-bromophenyl)-2-isopropyl-5-(4-phenylpiperazine-1-yl)pentanoic acid methyl ester was obtained by drying the mixture with anhydrous sodium sulfate and removing the solvent at low pressures (69 mg, 42%).

후처리

  1. temperatureheated
  2. temperaturerefluxed for 3 hours
  3. filtrationthe precipitate was filtrated
  4. distillationdistilled
  5. extractionextracted with ethyl acetate and water
  6. washAfter the organic layer was washed with 1N HCl and saturated NaHCO3

출처 및 근거

ORD 기록
ord-5be30e553d664163ac3b72e36c175460
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939672B2

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