反应详情

温度

165 °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 0.40 g (2.90 mmol) of 3-methyl-4-methoxyaniline was heated, with stirring, in a 165° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ether (1 mL) was added. The crystals that developed were filtered and washed with 2 mL of ether; wt 0.109 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform and then ethyl acetate. The ethyl acetate eluent was concentrated to 3 mL volume. On cooling, pure crystals of product separated; wt 0.060 g; mp 218°-220° C.

1. temperaturewas heated
2. temperatureThe resulting solution was heated for 5 minutes
3. temperaturecooled to room temperature
4. filtrationThe crystals that developed were filtered
5. washwashed with 2 mL of ether
6. customThe solid was purified
7. customto remove dark colors by silica gel chromatography
8. washeluting with chloroform
9. concentrationThe ethyl acetate eluent was concentrated to 3 mL volume
10. temperatureOn cooling
11. custompure crystals of product separated