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4'-Hydroxyacetophenone → HCID 10061000, 화합물

HRID 1732484
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HRID 1732484 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][CH:3]=1.[Br:11][CH2:12][CH2:13][CH2:14]Br.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Br:11][CH2:12][CH2:13][CH2:14][O:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 74694'-HydroxyacetophenoneHCID 80011,3-DibromopropaneHCID 11430Potassium Carbonate

생성물 1

HCID 10061000HCID 10061000, 화합물수율 70.1%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

p-Hydroxyacetophenone (13.6 g.), 1,3-dibromopropane (121.2 g.) and potassium carbonate (15.8 g.) were dissolved in acetone (250 ml.), and the solution was refluxed under heating for 6 hours. After the reaction mixture was filtered, the acetone was removed by evaporation from the filtrate under reduced pressure to give an oily residue. The excess of 1,3-dibromopropane was removed by distillation from the oily residue under reduced pressure to give a residue, which was subjected to column chromatography on silica gel (20 g.). Elution was carried out with benzene and the fractions containing a desired compound were collected. The eluate was evaporated to dryness under reduced pressure to give p-(3-bromopropoxy)acetophenone (18 g.).

후처리

  1. temperaturethe solution was refluxed
  2. temperatureunder heating for 6 hours
  3. filtrationAfter the reaction mixture was filtered
  4. customthe acetone was removed by evaporation from the filtrate under reduced pressure
  5. customto give an oily residue
  6. customThe excess of 1,3-dibromopropane was removed by distillation from the oily residue under reduced pressure
  7. customto give a residue, which
  8. washElution
  9. additionthe fractions containing a desired compound
  10. customwere collected
  11. customThe eluate was evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-c8365c8601ba4b9da2e0285c323cf354
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04237305

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