Benzoyl chloride → 1-[4-(4-Benzoylpiperazin-1-yl)phenyl]ethanone

HRID 885861

反応式

HRID 885861 の反応式
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:10]1([C:16]2[CH:21]=[CH:20][C:19]([C:22](=[O:24])[CH3:23])=[CH:18][CH:17]=2)[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C(Cl)Cl>[C:1]([N:13]1[CH2:12][CH2:11][N:10]([C:16]2[CH:17]=[CH:18][C:19]([C:22](=[O:24])[CH3:23])=[CH:20][CH:21]=2)[CH2:15][CH2:14]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 7412Benzoyl chlorideHCID 97269Piperazin-4-ylacetophenone

生成物 1

HCID 12451881-[4-(4-Benzoylpiperazin-1-yl)phenyl]ethanone収率 90.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Benzoyl chloride (0.341 ml, 2.94 mmol) was added dropwise to a stirred mixture of 1-(4-piperazin-1-yl-phenyl)-ethanone (500 mg, 2.45 mmol) and TEA (0.681 ml, 4.9 mmol) in DCM (25 ml). The resulting solution was stirred overnight at room temperature, then diluted with DCM and washed with water, with NaHCO3 (5% in H2O) and finally with citric acid (20% in H2O). The organic phase was dried over Na2SO4 and evaporated in vacuo. The resulting solid was triturated with di-isopropylether and filtered to give 687 mg of 1-[4-(4-benzoyl-piperazin-1-yl)-phenyl]-ethanone.

後処理

  1. washwashed with water, with NaHCO3 (5% in H2O) and finally with citric acid (20% in H2O)
  2. dry with materialThe organic phase was dried over Na2SO4
  3. customevaporated in vacuo
  4. customThe resulting solid was triturated with di-isopropylether
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-56f1b21b68304fcba970fb832ef0771c
出典データセット
uspto-grants-2012_08
特許番号
US08242175B2

関連ノート

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