5-(3,4-Dimethoxyphenyl)-2-cyclohexen-1-one → 3-(3,4-Dimethoxyphenyl)cyclohexanone

HRID 1108757노트

반응식

HRID 1108757 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[CH2:16][C:15](=[O:17])[CH:14]=[CH:13][CH2:12]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[H][H].Cl.C(OCC)(=O)C>C(O)C.C(OCC)(=O)C.[C].[Pd]>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[CH2:12][CH2:13][CH2:14][C:15](=[O:17])[CH2:16]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

7

반응물 3

HCID 187841395-(3,4-Dimethoxyphenyl)-2-cyclohexen-1-oneHCID 21866389Hydrogen chloride-ethyl acetateHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 187841823-(3,4-Dimethoxyphenyl)cyclohexanone수율 98.6%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

5-(3,4-Dimethoxyphenyl)-2-cyclohexen-1-one (6.76 g) was dissolved in ethanol (100 ml), and 10% palladium-carbon (684 mg) was added thereto. After substituting the reaction vessel with hydrogen gas, hydrogen addition was effected for 30 minutes at normal pressure and room temperature. After the reaction, the catalyst was filtered off and the solvent was distilled off under reduced pressure to produce an oily substance which was dissolved in ethyl acetate (50 ml), and then 4 N HCl-ethyl acetate solution (2 ml) was added and the mixture was stirred at room temperature for 20 minutes. The solvent was distilled off under reduced pressure to produce crude crystals which were then washed with n-hexane to give 6.72 g of 3-(3,4-dimethoxyphenyl)cyclohexanone (98.5%).

후처리

  1. customAfter the reaction
  2. filtrationthe catalyst was filtered off
  3. distillationthe solvent was distilled off under reduced pressure
  4. customto produce an oily substance which
  5. distillationThe solvent was distilled off under reduced pressure
  6. customto produce crude crystals which
  7. washwere then washed with n-hexane

출처 및 근거

ORD 기록
ord-d3b8805eb9db490385840eebd55aeaee
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06069176

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