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Acetic Anhydride → HCID 13031642, Verbindung

HRID 1439381
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1439381
[CH3:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][CH:4]([OH:9])[O:3]1.[C:10](OC(=O)C)(=[O:12])[CH3:11]>N1C=CC=CC=1>[CH3:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][CH:4]([O:9][C:10](=[O:12])[CH3:11])[O:3]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 13011787HCID 13011787, Verbindung

Produkt 1

HCID 13031642HCID 13031642, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A 12.8 g quantity of 2-methyl-6-hydroxy-3-oxo-3,6-dihydro-2H-pyran and 25 ml of acetic anhydride are reacted in the presence of 12.5 ml of pyridine with stirring at room temperature for 4 hours. After the reaction, the mixture is concentrated, the residue is poured into ice water, and the mixture is extracted with 100 ml of ether. The ethereal layer is washed with an aqueous solution of sodium carbonate and then dried over magnesium sulfate. After removing the magnesium sulfate, the ethereal layer is concentrated, and the residue is distilled at a reduced pressure of 0.4 mm Hg to give 12.6 g of 2-methyl-6-acetoxy-3-oxo-3,6-dihydro-2H-pyran as a colorless liquid fraction at 80° to 83° C in a yield of 80%.

Aufarbeitung

  1. customAfter the reaction
  2. concentrationthe mixture is concentrated
  3. additionthe residue is poured into ice water
  4. extractionthe mixture is extracted with 100 ml of ether
  5. washThe ethereal layer is washed with an aqueous solution of sodium carbonate
  6. dry with materialdried over magnesium sulfate
  7. customAfter removing the magnesium sulfate
  8. concentrationthe ethereal layer is concentrated
  9. distillationthe residue is distilled at a reduced pressure of 0.4 mm Hg

Quellen und Nachweise

ORD-Eintrag
ord-25718068c7b944e3a0be902b5410be70
Quelldatensatz
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04059595

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