Reaktion #8794

Reaktionsgleichung

ethyl 3-(4-fluorophenyl)-3-oxopropionate

acetoamidine hydrochloride

potassium carbonate

→

target compound

Ausbeute 87.6%

4-(4-fluorophenyl)-6-hydroxy-2-methylpyrimidine

Ausbeute 87.6%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeInsolubles were separated from the reaction mixture
2. 2
   Waschenwashed with methanol
3. 3
   Temperaturunder reflux for 4 hours
4. 4
   Sonstigethe precipitated crystal was isolated by centrifugation
5. 5
   Waschenwashed with water
6. 6
   Sonstigedried

Vorschrift

8.7 kg of ethyl 3-(4-fluorophenyl)-3-oxopropionate, 11.7 kg of acetoamidine hydrochloride and 28.6 kg of potassium carbonate were stirred for 5 hours at about 50° C. in 34.5 kg of methanol. Insolubles were separated from the reaction mixture and washed with methanol, and the mother liquor and the washing were combined with water and neutralized with an 18% aqueous solution of hydrochloric acid. After neutralization, the crystal was ripened by stirring under reflux for 4 hours, and the precipitated crystal was isolated by centrifugation, washed with water, dried to obtain 7.4 kg of the target compound as a white crystal.

Quelle