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Hydrogen Peroxide → HCID 178504195, 화합물

HRID 1275540
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HRID 1275540 반응식
[OH:1][C:2]1[C:3](=[O:23])[C:4]2[C:9]([C:10](=[O:22])[C:11]=1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]C[Si](C)(C)C)=[CH:8][CH:7]=[CH:6][CH:5]=2.C(OC1C(=O)C2C(C(=O)C=1)=CC=CC=2)(=O)C1C=CC=CC=1.[CH3:45][Si:46](C(CCCCC)C(O)=O)([CH3:48])[CH3:47].C(=O)([O-])[O-].[Na+].[Na+].OO>O1CCOCC1.O.S([O-])([O-])(=O)=O.[Cu+2]>[OH:1][C:2]1[C:3](=[O:23])[C:4]2[C:9]([C:10](=[O:22])[C:11]=1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][Si:46]([CH3:48])([CH3:47])[CH3:45])=[CH:8][CH:7]=[CH:6][CH:5]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 784Hydrogen PeroxideHCID 10340Sodium CarbonateHCID 825051HCID 825051, 화합물HCID 22117156HCID 22117156, 화합물HCID 178504196HCID 178504196, 화합물

생성물 1

HCID 178504195HCID 178504195, 화합물

시약·촉매·용매 3

HCID 24462
Copper Sulfate
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

반응 조건

온도
70 °C

실험 절차

2-Hydroxy-3(6'-trimethylsilylhexyl)-1,4-naphthoquinone (337 mg, 1.02 mmol), prepared from 2-benzoyloxy-1,4-naphthoquinone and trimethylsilylheptanoic acid by the method of Example 1 followed by the method of Example 2, was dissolved in dioxane (2.5 ml) under nitrogen. Sodium carbonate (120 mg) in water (2.5 ml) was added followed by an excess of 30% (w/v) hydrogen peroxide (200 μl). The mixture was heated at 70° C. for 40 minutes during which time the reaction mixture turned from red to colourless. The reaction mixture was allowed to cool and 20% (w/v) copper sulphate solution (100 μl) was added and the solution stirred until bubbling ceased. 25% (w/v) sodium hydroxide solution (2 ml) and 20% (w/v) copper sulphate solution (5 ml) were then added and the reaction mixture heated at 70° C. for 30 minutes. The mixture was allowed to cool and acidified to pH 2 with 1N hydrochloric acid. The product was extracted into diethyl ether and the ether extract was then washed with brine, dried over anhydrous magnesium sulphate and concentrated in vacuo. The crude material was chromatographed using 5% diethyl ether/hexane as eluent to give 2-hydroxy-3(5'-trimethylsilylpentyl)-1,4-naphthoquinone (202 mg) which was recrystallised from hexane, m. pt. 73-75° C. NMR peaks at: 184.6, 181.4, 153.0, 134.8, 132.9, 132.7, 129.4, 126.7, 126.0, 124.8; 33.6, 27.9, 33.7, 23.2, 16.5; -1.7.

후처리

  1. temperatureto cool
  2. customuntil bubbling
  3. addition25% (w/v) sodium hydroxide solution (2 ml) and 20% (w/v) copper sulphate solution (5 ml) were then added
  4. temperaturethe reaction mixture heated at 70° C. for 30 minutes
  5. temperatureto cool
  6. extractionThe product was extracted into diethyl ether
  7. extractionthe ether extract
  8. washwas then washed with brine
  9. dry with materialdried over anhydrous magnesium sulphate
  10. concentrationconcentrated in vacuo
  11. customThe crude material was chromatographed

출처 및 근거

ORD 기록
ord-85ac3400b43e45179af89ef17936d9b5
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06162799

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