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

HRID 2366499

반응식

HRID 2366499 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

HCID 1381042-Acetyl-1,3-cyclohexanedione수율 59%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-411f976d5d964e97b0e5089fb4fd3785
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697744B2

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