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Sodium Acetate → HCID 24828929, 화합물

HRID 859183
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HRID 859183 반응식
[CH2:1]([O:3][C:4](=[O:26])[C:5](=[N:17][NH:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[Cl:25])[C:6](=[O:16])[CH:7](Br)[C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)[CH3:2].C([O-])(=O)C.[Na+]>CO.C1CCCCC1>[CH2:1]([O:3][C:4]([C:5]1[C:6]([OH:16])=[C:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[N:18]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:25])[N:17]=1)=[O:26])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 178472846HCID 178472846, 화합물

생성물 1

HCID 24828929HCID 24828929, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8078Cyclohexane용매

실험 절차

A mixture of 4-bromo4-(4-chloro-phenyl)-2-[(2-chloro-phenyl)-hydrazono]-3-oxo-butyric acid ethyl ester (12.1 g, 26 mmol) and sodium acetate (10.8 g, 130 mmol) in methanol (100 ml) was heated at reflux for 4 hours, cooled, concentrated in vacuo and the residue partitioned between ethyl acetate and water. The organic layer was washed with brine, dried (Na2SO4) and concentrated in vacuo to afford a solid. A slurry of this material in cyclohexane was heated to reflux and allowed to stir at ambient temperature for 2 hours, and filtered to afford the title compound (I-1d) as a yellow solid (I-1d), 6.5 g.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  3. temperaturecooled
  4. concentrationconcentrated in vacuo
  5. customthe residue partitioned between ethyl acetate and water
  6. washThe organic layer was washed with brine
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo
  9. customto afford a solid
  10. temperatureto reflux
  11. filtrationfiltered

출처 및 근거

ORD 기록
ord-026fa372fac247a7924b5b40ed071121
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07151097B2

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