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

HRID 1856458
ノート
印刷プレビュー

反応式

HRID 1856458 の反応式
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
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 70961-PhenylpiperazineHCID 8471TriethylamineHCID 23345044HCID 23345044、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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of triethylamine, the reaction mixture is heated for 6 hours to 100 ° C. After the reaction has ceased, the solvent is withdrawn at 40° under a high vacuum.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.

後処理

  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 customthe solvent is withdrawn at 40° under a high vacuum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

出典と根拠

ORDレコード
ord-023b593912de4be9a2dbb5527d61848f
出典データセット
uspto-grants-1980_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04219551

反応ノート

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