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4'-Hydroxyacetophenone → HCID 10061000、化合物

HRID 1732484
ノート
印刷プレビュー

反応式

HRID 1732484 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 10061000HCID 10061000、化合物収率 70.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-c8365c8601ba4b9da2e0285c323cf354
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04237305

反応ノート

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