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Dimethyl Sulfate → HCID 54346298, Verbindung

HRID 1699147
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1699147
[CH3:1][C:2](=[CH2:10])[CH2:3][C:4](=[N:8][OH:9])[C:5](=[O:7])[CH3:6].[C:11](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[CH3:11][O:9][N:8]=[C:4]([CH2:3][C:2]([CH3:1])=[CH2:10])[C:5](=[O:7])[CH3:6]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 73447335HCID 73447335, Verbindung

Produkt 1

HCID 54346298HCID 54346298, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel2×

Reaktionsbedingungen

Temperatur
23 °C

Versuchsvorschrift

141 g of 5-methylhex-5-ene-2,3-dione 3-oxime from Example 1 were dissolved in 750 ml of acetone and admixed with 165.6 g of potassium carbonate. 145 g of dimethyl sulfate in 100 ml of acetone were then added dropwise, and the mixture was stirred at 23° C. for 4 hours. The solvent was subsequently removed under reduced pressure, the residue was taken up with methyl tert-butyl ether/water and the aqueous phase was extracted repeatedly with methyl tert-butyl ether. The combined organic phases were washed with 15% strength ammonia solution and water and dried over sodium sulfate, and the solvent was removed under reduced pressure. This gave 141 g of the title compound as a yellow oil.

Aufarbeitung

  1. customThe solvent was subsequently removed under reduced pressure
  2. extractionthe aqueous phase was extracted repeatedly with methyl tert-butyl ether
  3. washThe combined organic phases were washed with 15% strength ammonia solution and water
  4. dry with materialdried over sodium sulfate
  5. customthe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-64a150342fba47eeb20074144e72e266
Quelldatensatz
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06344589B1

Notizen zur Reaktion

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