Acetic Acid → HCID 20254624, Verbindung

HRID 2412839Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2412839
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([C:14]1[C:19]([OH:20])=[C:18]([O:21][CH3:22])[C:17]([O:23][CH3:24])=[CH:16][C:15]=1[CH3:25])=O.Cl(O)(=O)(=O)=O.[H][H].[C:33](O)(=[O:35])[CH3:34]>[Pd]>[C:33]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:14]1[C:19]([OH:20])=[C:18]([O:21][CH3:22])[C:17]([O:23][CH3:24])=[CH:16][C:15]=1[CH3:25])(=[O:35])[CH3:34]

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 24247Perchloric AcidHCID 132762366-(11-Hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenolHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 20254624HCID 20254624, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23938PalladiumKatalysator

Versuchsvorschrift

To a solution of 6-(11-hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenol (14 g) in acetic acid (200 ml) are added 5% palladium-on-carbon (50% hydrous) (3 g) and 70% perchloric acid (0.1 ml), and catalytic reduction is carried out at atmospheric temperature and pressure. When the hydrogen has ceased to be absorbed, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The residue is extracted with dichloromethane and the dichloromethane layer is washed with a 5% aqueous solution of sodium hydrogen carbonate and dried over anhydrous magnesium sulfate. The solvent is then distilled off to obtain a colorless oil of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (15 g).

Aufarbeitung

  1. customto be absorbed
  2. filtrationthe catalyst is filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. extractionThe residue is extracted with dichloromethane
  5. washthe dichloromethane layer is washed with a 5% aqueous solution of sodium hydrogen carbonate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent is then distilled off

Quellen und Nachweise

ORD-Eintrag
ord-d2e8c95e4ee44144a89b5834af3bb39c
Quelldatensatz
uspto-grants-1985_01
Patentnummer
US04495104

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