4-Methoxy-gamma,gamma,3-trimethylbenzenebutanoic acid → HCID 12088903、化合物

HRID 1166640ノート

反応式

HRID 1166640 の反応式
[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]

参加物

3

反応物 1

HCID 222183274-Methoxy-gamma,gamma,3-trimethylbenzenebutanoic acid2 回

生成物 1

HCID 12088903HCID 12088903、化合物収率 54.1%

試薬・触媒・溶媒 1

HCID 6395Methanesulfonic Acid溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e412188fbf7745d5b6214b3d8a1d8d46
出典データセット
uspto-grants-2003_09
特許番号
US06613917B1

反応ノート

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