Methanol → Tetrahydropyran-4-ylacetic acid

HRID 129506

Reaktionsgleichung

Reaktionsgleichung von HRID 129506
CO.[OH-].[Na+].[O:5]1[CH2:10][CH2:9][CH:8]([CH2:11][C:12]([O:14]CC)=[O:13])[CH2:7][CH2:6]1>O>[O:5]1[CH2:10][CH2:9][CH:8]([CH2:11][C:12]([OH:14])=[O:13])[CH2:7][CH2:6]1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 2773412Ethyl tetrahydropyran-4-ylacetate

Produkt 1

HCID 2773575Tetrahydropyran-4-ylacetic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

20 ml of methanol, 10 ml of water and 1 g of sodium hydroxide were added to 0.9 g of ethyl 4-tetrahydropyranylacetate and agitated at 80° C. for 1 hour. The solvent was removed by distillation, to which water was added. After washing with ethyl acetate, a hydrochloric acid aqueous solution was added to the resultant aqueous phase to an extent of pH of 3, followed by extraction with chloroform under salting-out conditions and drying with anhydrous magnesium sulfate. This was removed by filtration and the solvent was distilled off, thereby obtaining 0.87 g of a crude intended compound.

Aufarbeitung

  1. customThe solvent was removed by distillation, to which water
  2. additionwas added
  3. washAfter washing with ethyl acetate
  4. additiona hydrochloric acid aqueous solution was added to the resultant aqueous phase to an extent of pH of 3
  5. extractionfollowed by extraction with chloroform under salting-out conditions
  6. dry with materialdrying with anhydrous magnesium sulfate
  7. customThis was removed by filtration
  8. distillationthe solvent was distilled off
  9. customobtaining 0.87 g of a crude intended compound

Quellen und Nachweise

ORD-Eintrag
ord-7d62b7bd29474bb0903850b8dad8c0a0
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05468740

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