4-Methoxy-gamma,gamma,3-trimethylbenzenebutanoic acid → HCID 12088903, 화합물

HRID 1166640노트

반응식

HRID 1166640 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([CH3:16])([CH3:15])[CH2:10][CH2:11][C:12]([OH:14])=O)=[CH:5][C:4]=1[CH3:17]>CS(O)(=O)=O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[C:6]([C:9]([CH3:16])([CH3:15])[CH2:10][CH2:11][C:12]2=[O:14])=[CH:5][C:4]=1[CH3:17]

참가 물질

3

반응물 1

HCID 222183274-Methoxy-gamma,gamma,3-trimethylbenzenebutanoic acid2회

생성물 1

HCID 12088903HCID 12088903, 화합물수율 54.1%

시약·촉매·용매 1

HCID 6395Methanesulfonic Acid용매

실험 절차

A solution of 4-(4-methoxy-3-methylphenyl)-4-methyl-pentanoic acid (Compound 5, 7.8 g, 33 mmol) and 150 mL of methanesulfonic acid was stirred at room temperature under an argon atmosphere for 24 h, then poured into ice, extracted three times with ethyl acetate, washed with NaHCO3 1N, brine, and dried over MgSO4, and filtered. The solvent was removed, and the residue was purified by flash chromatography (Hexane:Ethyl Acetate=4:1) to afford 3.9 g (54%) of the title compound as a yellow solid.

후처리

  1. additionpoured into ice
  2. extractionextracted three times with ethyl acetate
  3. washwashed with NaHCO3 1N, brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customThe solvent was removed
  7. customthe residue was purified by flash chromatography (Hexane:Ethyl Acetate=4:1)

출처 및 근거

ORD 기록
ord-e412188fbf7745d5b6214b3d8a1d8d46
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06613917B1

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