p-Toluenesulfonic acid monohydrate → HCID 18615089, Verbindung

HRID 565450

Reaktionsgleichung

Reaktionsgleichung von HRID 565450
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[OH2:15].[C:16]1([CH3:26])C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.C(O)CO>[CH2:16]1[O:15][C:1]([C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][CH:5]=2)([CH3:2])[O:3][CH2:26]1

Komponenten

5

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 600911Ethyl 4-acetylbenzoate

Produkt 1

HCID 18615089HCID 18615089, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 174Ethylene GlycolLösungsmittelHCID 1140TolueneLösungsmittel

Versuchsvorschrift

ethyl 4-acetyl-benzoate (9.61 g, a product of the firm Wako Pure Chemical Ind.) was dissolved in toluene (200 ml) under an argon atmosphere whereto ethylene glycol (20 ml) and p-toluenesulfonic acid hydrate (200 mg) were added, whereupon the mixture was refluxed with heating for 24 hours while dehydrating on a Dean-Stark apparatus. After cooling down to room temerature, the toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly, followed by drying and concentrating to dryness under reduced pressure, whereby the above-identified compound was obtained (12.76 g).

Aufarbeitung

  1. additionwere added, whereupon the mixture
  2. temperaturewas refluxed
  3. temperaturewith heating for 24 hours
  4. temperatureAfter cooling down to room temerature
  5. washthe toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly
  6. customby drying
  7. concentrationconcentrating to dryness under reduced pressure, whereby the above-identified compound
  8. customwas obtained (12.76 g)

Quellen und Nachweise

ORD-Eintrag
ord-4162c50c57c448d4880a91b9ace26986
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06172099B2

Verknüpfte Notizen

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