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p-Toluenesulfonic acid → N,N-dimethyl-2-(4-oxocyclohexyl)acetamide

HRID 243565
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반응식

HRID 243565 반응식
C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH3:12][N:13]([CH3:27])[C:14](=[O:26])[CH2:15][CH:16]1[CH2:25][CH2:24][C:19]2(OCC[O:20]2)[CH2:18][CH2:17]1>CC(C)=O>[CH3:27][N:13]([CH3:12])[C:14](=[O:26])[CH2:15][CH:16]1[CH2:25][CH2:24][C:19](=[O:20])[CH2:18][CH2:17]1
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참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 59442805N,N-dimethyl-2-(1,4-dioxaspiro[4.5]decan-8-yl)acetamide

생성물 1

HCID 59442836N,N-dimethyl-2-(4-oxocyclohexyl)acetamide수율 99.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

p-Toluenesulfonic acid (84 mg) is added to a solution of N,N-dimethyl-2-(1,4-dioxaspiro[4.5]decan-8-yl)acetamide (500 mg) in acetone (10 ml) and the mixture is heated under reflux for 3 hours. The solvent is removed under reduced pressure. The residue is dissolved in CH2Cl2 and washed with water. The organic layer is dried (Na2SO4) and filtered, and the solvent is removed under reduced pressure to give N,N-dimethyl-2-(4-oxocyclohexyl)acetamide (400 mg).

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. customThe solvent is removed under reduced pressure
  4. dissolutionThe residue is dissolved in CH2Cl2
  5. washwashed with water
  6. dry with materialThe organic layer is dried (Na2SO4)
  7. filtrationfiltered
  8. customthe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-51a304ae37d4451fb65828b5bd44e609
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653262B2

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