Reaktion #486169

Reaktionsgleichung

ethyl caproate

sodium

diethyl oxalate

sodium ethylate

→

desired product

Diethyl 2-butyl-3-oxo-butanedioate

Lösungsmittel

ethanol

ether

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   TemperaturThe mixture was refluxed for 15 minutes
3. 3
   Temperaturcooled down slightly
4. 4
   Temperaturat reflux for 3 hours and at 30° C. to 35° C. for 16 hours
5. 5
   Sonstigethe aqueous phase was separated
6. 6
   Sonstigeby decanting
7. 7
   Waschenwashed twice with ether
8. 8
   ExtraktionExtraction
9. 9
   Waschenthe combined organic phases were washed with water
10. 10
    Trocknenwith a saturated solution of sodium chloride, dried
11. 11
    Sonstigeevaporated to dryness

Vorschrift

100 ml of ether, then 13.55 ml of diethyl oxalate were added to a solution of sodium ethylate prepared by stirring 2.3 g of sodium and 150 ml of ethanol at 40° C. for one hour. The mixture was refluxed for 15 minutes, cooled down slightly and 50 ml of ethyl caproate were added. The mixture was stirred at reflux for 3 hours and at 30° C. to 35° C. for 16 hours. 50 ml of water were added and the aqueous phase was separated by decanting, washed twice with ether and acidified with 2N hydrochloric acid. Extraction was carried out 3 times with ether and the combined organic phases were washed with water, then with a saturated solution of sodium chloride, dried and evaporated to dryness to obtain 9.5 g of the desired product which was used as is for the following step.

Quelle