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1-Phenylpiperazine → 4-[4-Methoxy-3-[2-(4-phenyl-1-piperazinyl)ethoxy]phenyl]pyrrolidin-2-one

HRID 1856458
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HRID 1856458 반응식
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:13]2[CH2:17][NH:16][C:15](=[O:18])[CH2:14]2)[CH:8]=[CH:9][C:10]=1[O:11][CH3:12].[C:19]1([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(N(CC)CC)C>CN(C)C=O>[CH3:12][O:11][C:10]1[CH:9]=[CH:8][C:7]([CH:13]2[CH2:17][NH:16][C:15](=[O:18])[CH2:14]2)=[CH:6][C:5]=1[O:4][CH2:3][CH2:2][N:28]1[CH2:29][CH2:30][N:25]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:26][CH2:27]1
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참가 물질

5

반응물 3

HCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 23345044HCID 23345044, 화합물

생성물 1

HCID 30184524-[4-Methoxy-3-[2-(4-phenyl-1-piperazinyl)ethoxy]phenyl]pyrrolidin-2-one수율 15.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

20 mmol of 4-[3-(2-chloroethoxy)-4-methoxyphenyl]-2-pyrrolidone is dissolved in 50 ml. of dimethylformamide. After adding 22 mmol of 1-phenylpiperazine (95% strength) and 20 mmol of triethylamine, the reaction mixture is heated for 6 hours to 100 ° C. After the reaction has ceased, the solvent is withdrawn at 40° under a high vacuum. The residue is taken up in 50 ml. of ethyl acetate, washed with semisaturated sodium chloride solution, and the solvent, after drying over sodium sulfate, is distilled off under vacuum, thus obtaining in a 15.2% yield 4-{4-methoxy-3-[2-(4-phenylpiperazin-1-yl)ethoxy]-phenyl}-2-pyrrolidone, m.p. 140°-141°. The dihydrochloride, m.p. 219°-221°, is precipitated from ethereal hydrochloric acid.

후처리

  1. temperaturethe reaction mixture is heated for 6 hours to 100 ° C
  2. customthe solvent is withdrawn at 40° under a high vacuum
  3. washof ethyl acetate, washed with semisaturated sodium chloride solution
  4. dry with materialthe solvent, after drying over sodium sulfate
  5. distillationis distilled off under vacuum

출처 및 근거

ORD 기록
ord-023b593912de4be9a2dbb5527d61848f
출처 데이터셋
uspto-grants-1980_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04219551

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