反应详情

温度

170 °C

A mixture of 0.152 g (0.43 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8-pyrido[2,3-d]pyrimidin-7-one of Example 37 and 0.50 g (2.90 mmol) of 1-(4-aminobutyl)-4-methylpiperazine was heated with stirring in a 170° C. oil bath. After 2 minutes, solution was complete. After 2 hours, the solution was cooled to room temperature, and the dark gum was dissolved in 25 mL of ether. The solution was washed with 4×5 mL of water. Most of the color went into the water wash. The ether solution was dried over potassium carbonate, filtered, and concentrated to ca. 2 mL volume. The crystals that separated on inducement were filtered and washed with ether; wt 0.063 g; mp 130°-132° C.;

1. temperaturewas heated
2. waitAfter 2 hours
3. temperaturethe solution was cooled to room temperature
4. washThe solution was washed with 4×5 mL of water
5. washwash
6. dry with materialThe ether solution was dried over potassium carbonate
7. filtrationfiltered
8. concentrationconcentrated to ca. 2 mL volume
9. customThe crystals that separated on inducement
10. filtrationwere filtered
11. washwashed with ether