Reaktion #170703

Reaktionsgleichung

sodium hydrogen carbonate

sodium carbonate

itaconic acid

bromine

→

titled compound

Ausbeute 56.0%

Sodium 5-oxo-2,5-dihydrofuran-3-carboxylate

Ausbeute 56.0%

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigea temperature of the reaction solution below 45° C.
2. 2
   Temperaturthe mixture was heated to 55° C
3. 3
   workup.STIRRINGthe mixture was stirred for 20 minutes
4. 4
   workup.STIRRINGstirred for 1 hour
5. 5
   FiltrationThe precipitated solid was collected by filtration
6. 6
   Waschenwashed with cold water and ethanol
7. 7
   Sonstigedried under reduced pressure

Vorschrift

To a solution of itaconic acid (26.0 g) in water (35 ml) was added dropwise bromine (10.3 ml) at room temperature while keeping a temperature of the reaction solution below 45° C., and then the mixture was stirred at 30° C. for 15 minutes. To this reaction solution was added portionwise sodium hydrogen carbonate (33.6 g), and then the mixture was heated to 55° C. To this reaction solution was added dropwise a solution of sodium carbonate (10.6 g) in water (15 ml), and then the mixture was stirred for 20 minutes. This reaction solution was iced, and stirred for 1 hour. The precipitated solid was collected by filtration, washed with cold water and ethanol, and then dried under reduced pressure to give the titled compound (16.8 g).

Quelle