反应详情

A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37 and 0.50 g (2.70 mmol) of 1-(5-aminopentyl)-4-methylpiperazine was heated with stirring in a 180° C. to 185° C. oil bath. After 2 minutes, solution was complete. After 0.5 hour, the solution was cooled to room temperature, and 5 mL of water was added to precipitate a taffy-like gum. Decanted and triturated gum again with 5 mL of water. Decanted and took up gum into 35 mL of ether. The ether solution was washed with 2×50 mL of water, dried (potassium carbonate), and concentrated to 5 mL volume. Petroleum ether was added to slight turbidity. The crystals that separated on inducement were filtered and washed with 80% ether/petroleum ether; wt 0.060 g; mp 110°-112° C.;

1. temperaturewas heated
2. waitAfter 0.5 hour
3. customto precipitate a taffy-like gum
4. customDecanted
5. customtriturated gum again with 5 mL of water
6. customDecanted
7. washThe ether solution was washed with 2×50 mL of water
8. dry with materialdried (potassium carbonate)
9. concentrationconcentrated to 5 mL volume
10. additionPetroleum ether was added to slight turbidity
11. customThe crystals that separated on inducement
12. filtrationwere filtered
13. washwashed with 80% ether/petroleum ether