反应详情

温度

130 °C

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, 1.08 g (10.0 mmol) of 2-(aminomethyl)pyridine and 0.5 mL of dimethylformamide was heated with stirring in a 130° C. oil bath. After 2 minutes, solution was complete. After 2 hours, the excess amine and dimethylformamide were evaporated at reduced pressure. Ether (5 mL) was added to the residue. Crystals immediately developed. Water (5 mL) was added, and the entire mixture was filtered. The cake was washed 5 mL of ether, 5 mL of water, and then dried; wt 0.164 g. Recrystallization from ethyl acetate gave 0.075 g of pure product; mp 198°-201° C.

1. temperaturewas heated
2. waitAfter 2 hours
3. customthe excess amine and dimethylformamide were evaporated at reduced pressure
4. additionEther (5 mL) was added to the residue
5. additionWater (5 mL) was added
6. filtrationthe entire mixture was filtered
7. washThe cake was washed 5 mL of ether, 5 mL of water
8. customdried
9. customRecrystallization from ethyl acetate