反应详情

温度

180 °C

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (4.70 mmol) of 4-methylaniline was heated, with stirring, in a 180° C. oil bath. The resulting solution was heated for 10 minutes. Much of the excess 4-methylaniline was evaporated at reduced pressure. The remainder was dissolved in 1 mL of ethyl acetate. The crystals that separated from the dark solution were filtered and washed with 2 mL of ethyl acetate and then ether; wt 0.111 g. Recrystallization from ethyl acetate gave pure product; wt 0.050 g; mp 243°-245° C.

1. temperaturewas heated
2. temperatureThe resulting solution was heated for 10 minutes
3. customMuch of the excess 4-methylaniline was evaporated at reduced pressure
4. dissolutionThe remainder was dissolved in 1 mL of ethyl acetate
5. customThe crystals that separated from the dark solution
6. filtrationwere filtered
7. washwashed with 2 mL of ethyl acetate
8. customRecrystallization from ethyl acetate
9. customgave pure product