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Ammonium Acetate → 4-[2(4-Benzoyloxy-3,5-dimethoxyphenyl)-vinyl]-1-methylquinolinium iodide

HRID 1588199
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HRID 1588199 반응식
[C:1]([OH:9])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:10](=O)[C:11]1[CH:21]=[C:18]([O:19][CH3:20])[C:16](O)=[C:13]([O:14][CH3:15])[CH:12]=1.[I-:23].[CH3:24][N+:25]1[C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[C:28]([CH3:35])=[CH:27][CH:26]=1.C([O-])(=O)C.[NH4+]>C(O)C>[I-:23].[C:1]([O:9][C:16]1[C:13]([O:14][CH3:15])=[CH:12][C:11]([CH:10]=[CH:35][C:28]2[C:29]3[C:34](=[CH:33][CH:32]=[CH:31][CH:30]=3)[N+:25]([CH3:24])=[CH:26][CH:27]=2)=[CH:21][C:18]=1[O:19][CH3:20])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 517165Ammonium AcetateHCID 110769741,4-Dimethylquinolinium iodideHCID 86746982Syringaldehyde benzoate

생성물 1

HCID 678267874-[2(4-Benzoyloxy-3,5-dimethoxyphenyl)-vinyl]-1-methylquinolinium iodide수율 81%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of syringaldehyde benzoate (2e)(0.18 g, 0.63 mmol), 1,4-dimethylquinolinium iodide (0.18 g, 0.63 mmol) and ammonium acetate (0.15 g, 1.9 mmol) was dissolved in warm ethanol and heated under reflux. The solution rapidly turned yellow and within 15 min, yellow precipitate formed. The reaction was continued for a further 1 h and then filtered. The collected solid was washed with methanol to give (24e)(0.28 g, 81%) as a fine yellow powder, m.p. decomp.>250° C. (Found: C, 58.86; H, 4.25; N, 2.71. C27H24NO4I calc. C., 58.60; H, 4.37; N, 2.53%).

후처리

  1. temperatureheated
  2. temperatureunder reflux
  3. customyellow precipitate formed
  4. waitThe reaction was continued for a further 1 h
  5. filtrationfiltered
  6. washThe collected solid was washed with methanol

출처 및 근거

ORD 기록
ord-8602509ab8df4822af7238b0d3b8e043
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05221606

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