反应详情

A mixture of 0.226 g (0.58 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 (2.80 mmol) of 4-aminophenylacetic acid, methyl ester base was heated in a 160° C. to 165° C. oil bath. The resulting solution was heated for 10 minutes and cooled to room temperature. The solution was treated with 1 mL of glacial acetic acid to dissolve. Water (10 mL) was added to precipitate a gum. The mixture was decanted, and the remaining gum was dissolved in 20 mL of chloroform. The chloroform solution was washed with 25 mL of water, dried (magnesium sulfate), filtered, and concentrated. Purification was effected by silica gel chromatography eluting with chloroform and then with 50% hexane/ethyl acetate to obtain the fraction containing pure product. The eluent was concentrated to dryness to obtain a solid; wt 0.141 g.

1. temperaturewas heated in a 160° C. to 165° C. oil bath
2. temperatureThe resulting solution was heated for 10 minutes
3. dissolutionto dissolve
4. customto precipitate a gum
5. customThe mixture was decanted
6. dissolutionthe remaining gum was dissolved in 20 mL of chloroform
7. washThe chloroform solution was washed with 25 mL of water
8. dry with materialdried (magnesium sulfate)
9. filtrationfiltered
10. concentrationconcentrated
11. customPurification
12. washeluting with chloroform
13. customwith 50% hexane/ethyl acetate to obtain the fraction
14. additioncontaining pure product
15. concentrationThe eluent was concentrated to dryness
16. customto obtain a solid