反应详情

温度

160 °C

A mixture of 0.155 g (0.40 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 (4.00 mmol) of 5-amino-2-methoxypyridine was heated, with stirring, in a 160° C. oil bath. The resulting solution was heated for 10 minutes and cooled to room temperature. Water (10 mL) was added to precipitate a gum. The mixture was decanted, and the remaining gum was triturated with 5 mL of water. The brown solid that developed was filtered, washed well with water, and dried; wt 0.135 g. Purification was effected by silica gel chromatography eluting with chloroform and then with ethyl acetate to obtain the fraction containing pure product. The eluent was concentrated to 2 mL volume. The crystals that separated on inducement were filtered and washed with 0.2 mL of ethyl acetate and then 0.5 mL of ether; wt 0.045 g; mp 233°-235° C.

1. temperaturewas heated
2. temperatureThe resulting solution was heated for 10 minutes
3. temperaturecooled to room temperature
4. customto precipitate a gum
5. customThe mixture was decanted
6. customthe remaining gum was triturated with 5 mL of water
7. filtrationThe brown solid that developed was filtered
8. washwashed well with water
9. customdried
10. customPurification
11. washeluting with chloroform
12. customwith ethyl acetate to obtain the fraction
13. additioncontaining pure product
14. concentrationThe eluent was concentrated to 2 mL volume
15. customThe crystals that separated on inducement
16. filtrationwere filtered
17. washwashed with 0.2 mL of ethyl acetate