반응 #94998

반응 방정식

trichloroacetamidine

potassium carbonate

ethyl 2-chloroacetoacetate

→

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

수율 31.0%

용매

water

반응 조건

후처리

1. 1
   기타The aqueous solution was decanted from heavier tars
2. 2
   기타The precipitate that was formed
3. 3
   여과was filtered
4. 4
   세척washed
5. 5
   기타dried
6. 6
   기타to give 14.7 g (31% yield; mp 130°-145° C.) of crude product
7. 7
   기타An analytical sample recrystallized from cyclohexane

실험 절차

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.

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