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Acetone → 4-Allyloxybenzophenone

HRID 876070
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HRID 876070 반응식
[OH:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:22][C:23]([CH3:25])=O.C(Br)C=C>O>[CH2:25]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:14][CH:15]=1)[CH:23]=[CH2:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 180AcetoneHCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 143474-Hydroxybenzophenone

생성물 1

HCID 2579104-Allyloxybenzophenone수율 91.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To start with, a three-necked flask was charged with commercially available 4-hydroxybenzophenone (39.6 g) and potassium carbonate (28 g), followed by argon substitution. Subsequently, dehydrated acetone (120 ml) was added, followed by well stirring, and then allyl bromide (18.6 ml) was added. Stirring was performed at 60° C. for 8 hours. After that, the mixture was cooled to a room temperature, and pure water was added, followed by stirring. Extraction with diethylether (100 ml) was performed twice. Extraction-and-washing with a 10% NaOH solution (100 ml) was performed twice, followed by drying over sodium sulfate. The solvent was removed by using an evaporator to obtain a pale yellow residue. The residue was recrystallized from methanol, followed by suction filtration, and then drying in vacuum was performed to obtain 4-allyloxybenzophenone (hereinafter referred to as ABP) which was a pure product (weight: 43.7 g, yield: 91.9%).

후처리

  1. stirringStirring
  2. stirringby stirring
  3. extractionExtraction with diethylether (100 ml)
  4. extractionExtraction-
  5. wash-washing with a 10% NaOH solution (100 ml)
  6. dry with materialby drying over sodium sulfate
  7. customThe solvent was removed
  8. customan evaporator
  9. customto obtain a pale yellow residue
  10. customThe residue was recrystallized from methanol
  11. filtrationfollowed by suction filtration
  12. customdrying in vacuum

출처 및 근거

ORD 기록
ord-6465e18953624be38c81c6114da4c063
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08986488B2

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