反应详情

温度

134 °C

A mixture of 0.100 g (0.26 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.300 g (3.00 mmol) of cyclohexylamine was heated to the boiling point (134° C.). The resulting solution was heated at reflux for 2 minutes. Most of the excess amine was evaporated at reduced pressure. The remaining gum was dissolved in 2 mL of ethyl acetate hot. Petroleum ether (2 mL) was added, and the crystals that separated from the cooled solution were filtered and washed with water; wt 0.090 g. Recrystallization from ethyl acetate gave pure crystalline product; 0.048 g; mp 242°-244° C.

1. temperatureThe resulting solution was heated
2. temperatureat reflux for 2 minutes
3. customMost of the excess amine was evaporated at reduced pressure
4. dissolutionThe remaining gum was dissolved in 2 mL of ethyl acetate hot
5. additionPetroleum ether (2 mL) was added
6. customthe crystals that separated from the cooled solution
7. filtrationwere filtered
8. washwashed with water
9. customRecrystallization from ethyl acetate
10. customgave pure crystalline product