反应详情

温度

195 °C

A mixture of 0.134 g (0.33 mmol) of 6-(2,6-dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 68 and 0.500 g (5.40 mmol) of aniline was heated with stirring in a 195° C. oil bath to reflux. The resulting solution was maintained at reflux for 5 minutes. Most of the excess aniline was evaporated at reduced pressure. The residual gum was dissolved in 15 mL of ethyl acetate. After filtration of a relatively small amount of insoluble material, the solution was filtered through a layer of silica gel to remove violet color. The filtrate was concentrated to 2 mL volume. Petroleum ether was added until slight turbidity. The crystals that separated on inducement were filtered and washed with 50% ether/petroleum ether; wt 0.068 g; mp 223°-225° C.

1. temperaturewas heated
2. temperatureto reflux
3. temperatureThe resulting solution was maintained
4. temperatureat reflux for 5 minutes
5. customMost of the excess aniline was evaporated at reduced pressure
6. dissolutionThe residual gum was dissolved in 15 mL of ethyl acetate
7. filtrationAfter filtration of a relatively small amount of insoluble material
8. filtrationthe solution was filtered through a layer of silica gel
9. customto remove violet color
10. concentrationThe filtrate was concentrated to 2 mL volume
11. additionPetroleum ether was added until slight turbidity
12. customThe crystals that separated on inducement
13. filtrationwere filtered
14. washwashed with 50% ether/petroleum ether