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1-Phenylpiperazine → HCID 69961743, 화합물

HRID 1291409
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HRID 1291409 반응식
Cl[C:2]1[CH:30]=[CH:29][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]=[CH:15][C:16]3[N:25]([CH3:26])[C:24](=[O:27])[C:23]4[C:18](=[CH:19][CH:20]=[CH:21][C:22]=4[CH3:28])[N:17]=3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][N:3]=1.[C:31]1([N:37]2[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1>N1C=CC=CC=1>[CH3:26][N:25]1[C:24](=[O:27])[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][C:22]=2[CH3:28])[N:17]=[C:16]1[CH:15]=[CH:14][C:11]1[CH:12]=[CH:13][C:8]([C:6](=[O:7])[C:5]2[CH:29]=[CH:30][C:2]([N:40]3[CH2:41][CH2:42][N:37]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[CH2:38][CH2:39]3)=[N:3][CH:4]=2)=[CH:9][CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70961-PhenylpiperazineHCID 73470985HCID 73470985, 화합물

생성물 1

HCID 69961743HCID 69961743, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
90 °C

실험 절차

To a solution of 2-[2-[4-(6-chloronicotinoyl)-phenyl]vinyl]-3,5-dimethyl-4(3H)-quinazolinone (333 mg) in pyridine (5 ml) was added 1-phenylpiperazine (156 ml) and the mixture was stirred at 90° C. for 4 hours. This reaction mixture was concentrated and extracted with ethyl acetate. The organic layer was washed serially with water and saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (n-hexane: ethyl acetate (1:1)) to provide 162 mg of yellow powder.

후처리

  1. concentrationThis reaction mixture was concentrated
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed serially with water and saturated aqueous NaCl solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (n-hexane: ethyl acetate (1:1))

출처 및 근거

ORD 기록
ord-8c20dee825304c92bf7d4d865ef9d496
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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