Ethylene Glycol → Methyl 4,4-ethylenedioxy-3-methyl-butanoate

HRID 2051726Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2051726
[CH3:1][CH:2]([CH:8]=[O:9])[CH2:3][C:4]([O:6][CH3:7])=[O:5].[CH2:10](O)[CH2:11][OH:12].C1(C)C=CC(S(O)(=O)=O)=CC=1.C1C=CC=CC=1>CCOCC>[CH2:10]1[CH2:11][O:12][CH:8]([CH:2]([CH3:1])[CH2:3][C:4]([O:6][CH3:7])=[O:5])[O:9]1

Komponenten

6

Edukt 4

HCID 174Ethylene GlycolHCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 11804788Methyl 3-methyl-4-oxobutanoate

Produkt 1

HCID 20305753Methyl 4,4-ethylenedioxy-3-methyl-butanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture of methyl 3-methyl-4-oxo-butanoate (86.3 g), ethylene glycol (61.75 g, 0.996 m), p-toluenesulfonic acid (1 g) and benzene (700 ml) is refluxed under nitrogen for 16 hr. The resulting mixture is allowed to cool to room temperature and treated with ether (300 ml). The organic phase is washed with 5% sodium bicarbonate solution (100 ml), dried (Na2SO4) and evaporated in vacuo to give methyl 4,4-ethylenedioxy-3-methyl-butanoate as a crude product (63.2 g). This material is used directly in the next step.

Aufarbeitung

  1. temperatureis refluxed under nitrogen for 16 hr
  2. washThe organic phase is washed with 5% sodium bicarbonate solution (100 ml)
  3. dry with materialdried (Na2SO4)
  4. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c30988f0051a47189587616052ccb2d1
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04182717

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