反応 #310316

反応方程式

trichloroacetamidine

potassium carbonate

ethyl 2-chloroacetoacetate

water

→

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

収率 31.0%

溶媒

cyclohexane

反応条件

後処理

1. 1
   その他The aqueous solution was decanted from heavier tars
2. 2
   その他The precipitate that was formed
3. 3
   ろ過was filtered
4. 4
   洗浄washed
5. 5
   その他dried
6. 6
   その他to give 14.7 g (31% yield; mp 130°-145° C.) of crude product

実験手順

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.

出典