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Butyl bromide → 1-Butoxy-3,5-difluorobenzene

HRID 1741552
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HRID 1741552 반응식
Br[CH2:2][CH2:3][CH2:4][CH3:5].[F:6][C:7]1[CH:8]=[C:9]([OH:14])[CH:10]=[C:11]([F:13])[CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:2]([O:14][C:9]1[CH:8]=[C:7]([F:6])[CH:12]=[C:11]([F:13])[CH:10]=1)[CH2:3][CH2:4][CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 759283,5-Difluorophenol

생성물 1

HCID 190101831-Butoxy-3,5-difluorobenzene

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A solution of 1-bromobutane (11.0 g, 0.08 mol) in acetone (30 ml) was added dropwise to a stirred, refluxing mixture of 3,5-difluorophenol (9.1 g, 0.07 mol) and potassium carbonate (30 g, 0.2 mol) in acetone (200 ml). The stirred mixture was heated under reflux for 24 h (glc analysis revealed absence of starting material). The product was extracted into ether (twice), and the combined ethereal extracts were washed with water, 5% sodium hydroxide, water and dried (MgSO4). Most of the solvent was removed in vacuo, and after the removal of the final amount of solvent and the excess of 1-bromobutane at atmospheric pressure, the residue was distilled to yield a colourless liquid.

후처리

  1. temperaturerefluxing
  2. temperatureThe stirred mixture was heated
  3. temperatureunder reflux for 24 h (glc analysis revealed absence of starting material)
  4. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
  5. washwere washed with water, 5% sodium hydroxide, water
  6. dry with materialdried (MgSO4)
  7. customMost of the solvent was removed in vacuo
  8. customafter the removal of the final amount of solvent
  9. distillationthe excess of 1-bromobutane at atmospheric pressure, the residue was distilled
  10. customto yield a colourless liquid

출처 및 근거

ORD 기록
ord-5f9c616dc41a4fbdab9a8ecbb9042829
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05334327

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