Reaktion #2139905

Reaktionsgleichung

carbon dioxide

5-fluoro-orotic acid monohydrate

water

→

5-fluorouracil

Ausbeute 90.0%

Lösungsmittel

triethyleneglycol dimethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Sonstigehigher than 130° C.
3. 3
   Sonstigehigher than 190° C
4. 4
   TemperaturAfter cooling the reaction mixture
5. 5
   Sonstigethe reaction product was separated by a filtration
6. 6
   Sonstigerecrystallized from water

Vorschrift

In the example, 20 g of crystals of 5-fluoro-orotic acid monohydrate obtained by the fluorination and the post-treatment of Example 1 was suspended in 80 ml of triethyleneglycol dimethyl ether and the mixture was heated under stirring whereby water was generated at higher than 130° C. and carbon dioxide was generated at higher than 190° C. The decarboxylation was completed by heating at 200° C. for about 20 minutes. After cooling the reaction mixture, the reaction product was separated by a filtration and recrystallized from water to obtain 12.2 g of 5-fluorouracil. The yield was 90% based on 5-fluoro-orotic acid monohydrate.

Quelle