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

HRID 1795577ノート

反応式

HRID 1795577 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 1 N, 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 1 N, 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-31b880db4c264fd9ba41b3b554158a5c
出典データセット
uspto-grants-2006_04
特許番号
US07026487B2

反応ノート

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