Reaktion #310316

Reaktionsgleichung

trichloroacetamidine

potassium carbonate

ethyl 2-chloroacetoacetate

water

→

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

Ausbeute 31.0%

Lösungsmittel

cyclohexane

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

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 was prepared by recrystallization from cyclohexane (mp 156°-157° C.). The structure was confirmed via infrared and elemental analysis.

Quelle