反応 #95000
ord-332f755aa4f94c26b724fcd1f0380f00
反応方程式
trichloroacetamidine
potassium carbonate
ethyl-4-chloroacetoacetate
→
crude product
収率 36.1%
6-Chloromethyl-4-Hydroxy-2-Trichloromethylpyrimidine
収率 36.1%
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1ろ過The aqueous solution was filtered
- 2その他to give a precipitate
- 3洗浄The precipitate was washed
- 4その他dried
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-4-chloroacetoacetate and 400 ml water was stirred 18 hours. The aqueous solution was filtered and acidified with hydrochloric acid to give a precipitate. The precipitate was washed and dried to give 17.0 g (36% yield) of crude product. An analytical sample recrystallized from ligroin had mp 138°-144° C. The structure was confirmed via infrared and elemental analysis.