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Sodium Hydroxide → 2,2,5,5-Tetramethyl-3,4-hexanedione

HRID 2367864
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HRID 2367864 반응식
[CH3:1][C:2]([CH3:12])([C:4](=[O:11])[CH:5]([OH:10])[C:6]([CH3:9])([CH3:8])[CH3:7])[CH3:3].[Mn]([O-])(=O)(=O)=O.[K+].[OH-].[Na+]>CCCCCC>[CH3:8][C:6]([CH3:9])([C:5](=[O:10])[C:4](=[O:11])[C:2]([CH3:12])([CH3:3])[CH3:1])[CH3:7]
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 2195934-Hydroxy-2,2,5,5-tetramethylhexan-3-oneHCID 516875Potassium Permanganate

생성물 1

HCID 1382182,2,5,5-Tetramethyl-3,4-hexanedione수율 82.2%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

7.8 g (0.045 moles) of 2,2,5,5-tetramethyl-4-hydroxy-3-hexanone were dissolved in 90 ml of hexane and stirred vigorously with 157 ml of 1M aqueous potassium permanganate solution containing 1.8 g (0.045 moles) of sodium hydroxide. This mixture was then refluxed overnight. The mixture was then cooled to room temperature and the hexane layer separated. The aqueous layer was then extracted three times with 50 ml of hexane. The hexane solutions were then combined and washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate. The mixture was then filtered and the hexane distilled off at atmospheric pressure to yield 6.3 g of 2,2,5,5-tetramethyl-3,4-hexanedione (82% of theoretical).

후처리

  1. temperatureThis mixture was then refluxed overnight
  2. customthe hexane layer separated
  3. extractionThe aqueous layer was then extracted three times with 50 ml of hexane
  4. washwashed three times with 50 ml of pure water
  5. dry with materialbefore drying over anhydrous magnesium sulfate
  6. filtrationThe mixture was then filtered
  7. distillationthe hexane distilled off at atmospheric pressure

출처 및 근거

ORD 기록
ord-cf1e82c912544c77948ee3700f6d3928
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703103B2

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