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Hydrogen Peroxide → HCID 178504195, Verbindung

HRID 1275540
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1275540
[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
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 784Hydrogen PeroxideHCID 10340Sodium CarbonateHCID 825051HCID 825051, VerbindungHCID 22117156HCID 22117156, VerbindungHCID 178504196HCID 178504196, Verbindung

Produkt 1

HCID 178504195HCID 178504195, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel

3
HCID 24462Copper SulfateKatalysatorHCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-85ac3400b43e45179af89ef17936d9b5
Quelldatensatz
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06162799

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