反应详情

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.

1. customThe aqueous solution was decanted from heavier tars
2. customThe precipitate that was formed
3. filtrationwas filtered
4. washwashed
5. customdried
6. customto give 14.7 g (31% yield; mp 130°-145° C.) of crude product
7. customAn analytical sample recrystallized from cyclohexane