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Acetic Acid → 1-(2,4-Dihydroxy-5-isobutyl-phenyl)-ethanone

HRID 2097297
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인쇄 미리보기

반응식

HRID 2097297 반응식
[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:6]=1[OH:12])[CH:2]([CH3:4])[CH3:3].B(F)(F)F.[CH3:17][CH2:18][O:19]CC.C(O)(=O)C.CC([O-])=O.[Na+]>>[OH:11][C:8]1[CH:7]=[C:6]([OH:12])[C:5]([CH2:1][CH:2]([CH3:4])[CH3:3])=[CH:10][C:9]=1[C:18](=[O:19])[CH3:17]
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참가 물질

5

반응물 4

HCID 176Acetic AcidHCID 8000Boron trifluoride etherateHCID 517045Sodium AcetateHCID 139510854-Isobutylresorcinol

생성물 1

HCID 592647801-(2,4-Dihydroxy-5-isobutyl-phenyl)-ethanone

반응 조건

온도
90 °C

실험 절차

4-Isobutyl-benzene-1,3-diol (1 eq) was taken up in BF3.OEt2 (6 eq) and acetic acid (2 eq) was added. The solution was heated for 16 hours at 90° C. than allowed to cool to room temperature. The solution was added drop wise to 10% NaOAc (aq) and allowed to stand for 4 hours, before being extracted twice with diethyl ether. The organic phases were combined and washed with sat. NaHCO3 (aq), then dried over magnesium sulfate, filtered and concentrated in vacuo to give 1-(2,4-dihydroxy-5-isobutyl-phenyl)-ethanone, which was used without additional purification.

후처리

  1. temperatureto cool to room temperature
  2. extractionbefore being extracted twice with diethyl ether
  3. washwashed with sat. NaHCO3 (aq)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-61cd99a26c8b41a88026c030debdb936
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08450310B2

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