Oxygen → 3,5-Octanedione

HRID 132722

Reaktionsgleichung

Reaktionsgleichung von HRID 132722
O=O.[H-].[Na+].[C:5]([O:10]CC)(=O)[CH2:6][CH2:7][CH3:8].[CH3:13][C:14](=[O:17])[CH2:15][CH3:16]>N#N.O1CCCC1.O>[CH3:16][CH2:15][C:14](=[O:17])[CH2:13][C:5](=[O:10])[CH2:6][CH2:7][CH3:8]

Komponenten

8

Edukt 4

HCID 977OxygenHCID 6569Methyl Ethyl KetoneHCID 7762Ethyl butyrateHCID 24758Sodium hydride

Produkt 1

HCID 806023,5-OctanedioneAusbeute 56,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 947NitrogenLösungsmittelHCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In N2 atmosphere free of water and oxygen, to a 3-neck flask placed in an ice-bath and equipped with addition funnel and reflux condenser were successively added 0.07 mol sodium hydride and 100 ml tetrahydrofuran. To the mixture was added dropwise a solution of 0.06 mol ethyl butyrate and 0.03 mol butanone with stirring. Upon completing the addition, the mixture was heated refluxing for 4 hours. The solvent and composition with a boiling point below 110° C. were removed by distillation. To the residue was added an appropriate amount of saturated saline until the solid composition was just dissolved. The mixture was extracted with ethyl ether for three times. The organic phases were combined and dried over anhydrous sodium sulfate. The solvent was removed by distillation to give 2.4 g product.

Aufarbeitung

  1. customequipped with addition funnel
  2. temperaturereflux condenser
  3. additionthe addition
  4. temperaturethe mixture was heated
  5. temperaturerefluxing for 4 hours
  6. customThe solvent and composition with a boiling point below 110° C. were removed by distillation
  7. additionTo the residue was added an appropriate amount of saturated saline until the solid composition
  8. dissolutionwas just dissolved
  9. extractionThe mixture was extracted with ethyl ether for three times
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was removed by distillation

Quellen und Nachweise

ORD-Eintrag
ord-09f630a0eeb34a17823d5df51424f236
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07388061B2

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