反应详情

温度

110 °C

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.

1. temperaturewas heated
2. temperatureAfter 20 hours reflux
3. customthe excess amine and dimethylformamide were evaporated
4. customthe residue was triturated with water
5. filtrationfiltered
6. washwashed with water
7. customdried
8. customRecrystallization from ethyl acetate/petroleum ether
9. customgave pure product