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

HRID 885861

반응식

HRID 885861 반응식
[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

참가 물질

4

반응물 2

HCID 7412Benzoyl chlorideHCID 97269Piperazin-4-ylacetophenone

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-56f1b21b68304fcba970fb832ef0771c
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242175B2

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