Ethanol → Diethyl 2,2-dimethylglutarate

HRID 132742

Reaktionsgleichung

Reaktionsgleichung von HRID 132742
[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8]([OH:10])=[O:9])[C:3]([OH:5])=[O:4].[CH2:12](O)[CH3:13].[C:15]1(C)C=CC=C[CH:16]=1.S(=O)(=O)(O)O>O>[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8]([O:10][CH2:12][CH3:13])=[O:9])[C:3]([O:5][CH2:15][CH3:16])=[O:4]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 1140TolueneHCID 126812,2-Dimethylglutaric acid

Produkt 1

HCID 550221Diethyl 2,2-dimethylglutarateAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 0.1 mol 2,2-dimethyl-glutaric acid were added 0.3 mol ethanol, 40 ml toluene, and 0.4 ml concentrated sulfuric acid with stirring. The mixture was heated refluxing, and the water produced was removed by using a water separator until the amount of the water separated reached theoretical value. The mixture was neutralized with saturated sodium carbonate solution and extracted with ethyl acetate. The upper layer solution was separated, washed with saturated saline until being neutral, and dried over anhydrous sodium sulfate. After the solvent was removed, distillation under reduced pressure gave diethyl 2,2-dimethylglutarate as a colorless liquid, and the yield was 90%.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperaturerefluxing
  3. customwas removed
  4. customseparated
  5. extractionextracted with ethyl acetate
  6. customThe upper layer solution was separated
  7. washwashed with saturated saline
  8. dry with materialdried over anhydrous sodium sulfate
  9. customAfter the solvent was removed
  10. distillationdistillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e5342c668a2146d48d412a1ba6d23ca5
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07388061B2

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