Perchloric Acid → Benzenebutanoic acid, 4-cyclohexyl-

HRID 861865ノート

反応式

HRID 861865 の反応式
[CH:1]1([C:7]2[CH:19]=[CH:18][C:10]([C:11]([CH2:13][CH2:14][C:15]([OH:17])=[O:16])=O)=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl(O)(=O)(=O)=O>[C].[Pd].C(O)(=O)C>[CH:1]1([C:7]2[CH:8]=[CH:9][C:10]([CH2:11][CH2:13][CH2:14][C:15]([OH:17])=[O:16])=[CH:18][CH:19]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

5

反応物 2

HCID 24247Perchloric AcidHCID 1618624-(4-Cyclohexylphenyl)-4-oxobutanoic acid

生成物 1

HCID 3041568Benzenebutanoic acid, 4-cyclohexyl-収率 102.7%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 176Acetic Acid溶媒

実験手順

A solution of 3-(4-cyclohexylbenzoyl)propionic acid (10.7 g), acetic acid (100 ml) and perchloric acid (2.3 ml) was hydrogenated in the presence of 5% palladium carbon (50% wet, 3.0g) at room temperature under ordinary pressure. After removal of the catalyst by filtration, the filtrate was concentrated under reduced pressure. After water (100 ml) was added, the residue was extracted with ethyl acetate. The ethyl acetate layer was washed with water and brine, and dried (MgSO4), after which the solvent was evaporated off, to yield 4-(4-cyclohexylphenyl)butyric acid (10.4 g, 100%) as an oil.

後処理

  1. customAfter removal of the catalyst
  2. filtrationby filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionAfter water (100 ml) was added
  5. extractionthe residue was extracted with ethyl acetate
  6. washThe ethyl acetate layer was washed with water and brine
  7. dry with materialdried (MgSO4)
  8. customafter which the solvent was evaporated off

出典と根拠

ORDレコード
ord-8ad57db0acd24620ae9ed08cdc327bd0
出典データセット
uspto-grants-1998_02
特許番号
US05716944

反応ノート

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