Sulfuric Acid → 2-Acetyl-1,3-cyclohexanedione

HRID 2366499

反応式

HRID 2366499 の反応式
[Al+3].[Cl-].[Cl-].[Cl-].C([O:8][C:9]1[CH2:14][CH2:13][CH2:12][C:11](=[O:15])[CH:10]=1)(=O)C.[OH:16]S(O)(=O)=O.Cl[CH:22](Cl)[CH3:23]>>[C:22]([CH:10]1[C:11](=[O:15])[CH2:12][CH2:13][CH2:14][C:9]1=[O:8])(=[O:16])[CH3:23]

参加物

5

反応物 4

HCID 1118Sulfuric AcidHCID 63651,1-DichloroethaneHCID 27554433-Acetoxy-2-cyclohexen-1-oneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 1381042-Acetyl-1,3-cyclohexanedione収率 59%

実験手順

According to Scheme 4 Step 2: AlCl3 (26.5 mmol, 3.53 g) was added to a solution of 3-oxocyclohex-1-enyl acetate (13.2 mmol, 2.04 g) in dichloroethane (10 mL) and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was poured onto a solution of H2SO4 in ice. The aqueous phase was extracted with CHCl3 (50 mL). The organic phase was washed with water, dried over Na2SO4, was filtered and was concentrated to yield 2-acetylcyclohexane-1,3-dione (7.78 mmol, 1.20 g, 59%) as a yellow oil.

後処理

  1. extractionThe aqueous phase was extracted with CHCl3 (50 mL)
  2. washThe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. filtrationwas filtered
  5. concentrationwas concentrated

出典と根拠

ORDレコード
ord-411f976d5d964e97b0e5089fb4fd3785
出典データセット
uspto-grants-2014_04
特許番号
US08697744B2

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