Reaktion #50439

Reaktionsgleichung

3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

potassium fluoride

18-crown-6

→

7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-fluoro-phthalide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux temperature for 100 minutes
2. 2
   FiltrationThe mixture is then filtered over Celite®
3. 3
   Einengenis concentrated by evaporation
4. 4
   Sonstigethe crude product is recrystallised from ethyl acetate/n-hexane

Vorschrift

A mixture of 1.0 g of 3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see Example 85) and 0.19 g of spray-dried potassium fluoride and a spatula tip of 18-crown-6 is heated at reflux temperature for 100 minutes. The mixture is then filtered over Celite® and is concentrated by evaporation, and the crude product is recrystallised from ethyl acetate/n-hexane to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-fluoro-phthalide, m.p. 172°-174° C.

Quelle