Hydrochloric Acid → HCID 12832654, Verbindung

HRID 1903430Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1903430
C([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[C:21](=[O:22])[C:20]([O:23][CH3:24])=[C:19]([O:25][CH3:26])[C:18](=[O:27])[C:17]=1[CH3:28])(=O)C.Cl.C(=O)(O)[O-].[Na+]>CO>[OH:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[C:21](=[O:22])[C:20]([O:23][CH3:24])=[C:19]([O:25][CH3:26])[C:18](=[O:27])[C:17]=1[CH3:28]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 128326536-(11-Acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone

Produkt 1

HCID 12832654HCID 12832654, VerbindungAusbeute 95,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution (200 ml) of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.2 g) in methanol is added concentrated hydrochloric acid (0.1 ml), and the mixture is allowed to stand at room temperature for 12 hours. To the reaction mixture is added sodium bicarbonate (0.2 g) and the solvent is distilled off. The product is dissolved in dichloromethane and the insoluble matter is filtered off. Removal of dichloromethane by distillation gives crude crystals. Recrystallization from hexane-ether (3:1) yields orange-yellow needles of 6-(11-hydroxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (I, n=11) (3.6 g) m.p. 57° C.

Aufarbeitung

  1. distillationthe solvent is distilled off
  2. dissolutionThe product is dissolved in dichloromethane
  3. filtrationthe insoluble matter is filtered off
  4. customRemoval of dichloromethane
  5. distillationby distillation
  6. customgives crude crystals
  7. customRecrystallization from hexane-ether (3:1)

Quellen und Nachweise

ORD-Eintrag
ord-7ff19dfbb3b9447b8d1f941be238ccc2
Quelldatensatz
uspto-grants-1984_03
Patentnummer
US04436753

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