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

HRID 243565
ノート
印刷プレビュー

反応式

HRID 243565 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-51a304ae37d4451fb65828b5bd44e609
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08653262B2

反応ノート

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