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Phosphorus oxychloride → HCID 68780328, 화합물

HRID 2266444
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HRID 2266444 반응식
[CH3:1][O:2][C:3](=[O:27])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]2[C:7]=1[C:8](=O)[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)=[C:10]([CH3:17])[NH:11]2.C([O-])(=O)C.[Na+].P(Cl)(Cl)([Cl:35])=O>>[CH3:1][O:2][C:3](=[O:27])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]2[C:7]=1[C:8]([Cl:35])=[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)[C:10]([CH3:17])=[N:11]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 517045Sodium AcetateHCID 68782520HCID 68782520, 화합물

생성물 1

HCID 68780328HCID 68780328, 화합물

실험 절차

A solution of [8-chloro-3-(4-chlorobenzyl)-2-methyl-4-oxo-1,4-dihydroquinolin-5-yloxy]acetic acid methyl ester (0.13 g) in phosphorus oxychloride (5.0 mL) was heated at 180° C. in a microwave reactor for 15 minutes. The mixture was poured into ice and the pH of the solution adjusted to 3 by the addition of sodium acetate. The mixture was extracted with ethyl acetate and the combined extracts washed with saturated aqueous sodium hydrogen carbonate solution and dried over magnesium sulfate. The solvent removed under reduced pressure to afford title compound as a beige solid, 0.12 g.

후처리

  • additionThe mixture was poured into ice
  • extractionThe mixture was extracted with ethyl acetate
  • washthe combined extracts washed with saturated aqueous sodium hydrogen carbonate solution
  • dry with materialdried over magnesium sulfate
  • customThe solvent removed under reduced pressure
  • 출처 및 근거

    ORD 기록
    ord-8c4732f1a97245f0a356e7a8dc6d6c04
    출처 데이터셋
    uspto-grants-2010_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07858640B2

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