反应详情

温度

150 °C

A mixture of 0.155 g (0.40 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one, 0.167 g (0.80 mmol) of 4-(2-diethylaminoethoxy)aniline and 1 mL of (2-methoxyethyl)ether (bp 162° C.) was heated with stirring in a 150° C. oil bath. All solid gradually dissolved over a period of 10 minutes. The solution was heated another 10 minutes and cooled to 100° C. Water was added dropwise until slight turbidity. The crystals that separated on inducement were filtered, washed with 0.5 mL of ether and 2 mL of water, and dried; wt 0.105 g. Purification was effected by chromatography eluting with chloroform, then ethyl acetate and finally 10% methanol/chloroform to obtain fraction with pure product. The eluent was evaporated to dryness. The remaining amorphous solid was dissolved in 1 mL of warm ethyl acetate. The crystals that separated on inducement were filtered and washed sparingly with ethyl acetate and ether; wt 0.042 g; mp 141-143° C.

1. temperaturewas heated
2. dissolutionAll solid gradually dissolved over a period of 10 minutes
3. temperatureThe solution was heated another 10 minutes
4. temperaturecooled to 100° C
5. customThe crystals that separated on inducement
6. filtrationwere filtered
7. washwashed with 0.5 mL of ether and 2 mL of water
8. customdried
9. customPurification
10. washeluting with chloroform
11. customethyl acetate and finally 10% methanol/chloroform to obtain fraction with pure product
12. customThe eluent was evaporated to dryness
13. dissolutionThe remaining amorphous solid was dissolved in 1 mL of warm ethyl acetate
14. customThe crystals that separated on inducement
15. filtrationwere filtered
16. washwashed sparingly with ethyl acetate and ether