Piperazine → HCID 46186740、化合物

HRID 547984

反応式

HRID 547984 の反応式
[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

参加物

7

反応物 5

HCID 4837PiperazineHCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 23675764Sodium IodateHCID 46855860HCID 46855860、化合物

生成物 1

HCID 46186740HCID 46186740、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5be30e553d664163ac3b72e36c175460
出典データセット
uspto-grants-2011_05
特許番号
US07939672B2

関連ノート

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