反応 #3282
ord-a8f31c3f69e44f889459e4fbf80bb158
反応方程式
反応物
試薬
なし
反応条件
温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度was heated
- 2温度After 20 hours reflux
- 3その他the excess amine and dimethylformamide were evaporated
- 4その他the residue was triturated with water
- 5ろ過filtered
- 6洗浄washed with water
- 7その他dried
- 8その他Recrystallization from ethyl acetate/petroleum ether
- 9その他gave pure product
実験手順
A mixture of 0.177 g (0.50 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 10 mL of n-butylamine and 1.0 mL of dimethylformamide was heated with stirring to reflux (110° C. oil bath). After 1 hour, solution was complete. After 20 hours reflux, the excess amine and dimethylformamide were evaporated, and the residue was triturated with water, filtered, washed with water, and dried; wt 0.180 g. Recrystallization from ethyl acetate/petroleum ether gave pure product; wt 0.116 g; mp 184°-186° C.