Diethyl Carbonate → 5,5-Dimethyl-1,3-dioxan-2-one

HRID 1263316

Reaktionsgleichung

Reaktionsgleichung von HRID 1263316
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH2:3][OH:4].[C:8](=O)(OCC)[O:9]CC.O(C)[Na]>>[CH3:1][C:2]1([CH3:7])[CH2:5][O:6][C:8](=[O:9])[O:4][CH2:3]1

Komponenten

4

Edukt 3

HCID 7766Diethyl CarbonateHCID 31344Neopentyl glycolHCID 178418582HCID 178418582, Verbindung

Produkt 1

HCID 1379845,5-Dimethyl-1,3-dioxan-2-one

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of 208 grams (2 moles) 2,2-dimethyl-1,3-propanediol (neopentyl glycol), 295 grams diethyl carbonate, and 4.3 grams NaOCH3 was placed in a flask equipped with an 18-inch vigreux column and heated gradually to 130° C. About 230 ml ethanol was distilled. When the pot temperature reached 150°-160° C. excess diethyl carbonate was removed under reduced pressure. The resulting product was dissolved in benzene, washed with water, and concentrated. This product was recrystallized from ether and isolated as pure 5,5-dimethyl-1,3-dioxan-2-one. A 75 gram sample had a melting point of 108° C., very nearly matching that in the literature (109° C.).

Aufarbeitung

  1. customwas placed in a flask
  2. customequipped with an 18-inch vigreux column
  3. distillationAbout 230 ml ethanol was distilled
  4. customreached 150°-160° C.
  5. customwas removed under reduced pressure
  6. dissolutionThe resulting product was dissolved in benzene
  7. washwashed with water
  8. concentrationconcentrated
  9. customThis product was recrystallized from ether

Quellen und Nachweise

ORD-Eintrag
ord-aced9a31e8484aedb1bce44139dad808
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04456745

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