Reaktion #938092

Reaktionsgleichung

trichloroacetamidine

potassium carbonate

ethyl-2-chloroacetoacetate

→

5-Chloro-4-Hydroxy-6-Methyl-2-Trichloromethylpyrimidine

Ausbeute 31.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe aqueous solution was decanted from heavier tars
2. 2
   SonstigeThe precipitate that was formed
3. 3
   Filtrationwas filtered
4. 4
   Waschenwashed
5. 5
   Sonstigedried
6. 6
   Sonstigeto give 14.7 g (31% yield; mp 130°-145° C.) of crude product
7. 7
   SonstigeAn analytical sample recrystallized from cyclohexane

Vorschrift

A mixture of 30.0 g (0.18 mole) trichloroacetamidine, 25.2 g (0.18 mole) potassium carbonate, 30.3 g (0.18 mole) ethyl-2-chloroacetoacetate, and 300 ml water was stirred 18 hours. The aqueous solution was decanted from heavier tars and acidified with hydrochloric acid. The precipitate that was formed, was filtered, washed, and dried to give 14.7 g (31% yield; mp 130°-145° C.) of crude product. An analytical sample recrystallized from cyclohexane had mp 156°-157° C. The structure was confirmed via infrared and elemental analysis.

Quelle