反应详情

温度

210 °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, 0.500 g (5.30 mmol) of 3-aminopyridine base, and 0.066 g (0.50 mmol) of 3-aminopyridine hydrochloride was heated with stirring in a 210° C. oil bath for 1 hour. Water (5 mL) was added to the cooled reaction mixture to precipitate a solid. The solid was filtered, washed well with water, and dried; wt 0.147 g. Purification was effected by silica gel chromatography by eluting with chloroform and then ethyl acetate. The ethyl acetate eluent containing the pure product was concentrated to 2 mL volume. The crystals that separated on inducement were filtered and washed with 0.5 mL of ethyl acetate and 1 mL of ether; wt 0.810 g; mp 247°-248° C.

1. temperaturewas heated
2. customto precipitate a solid
3. filtrationThe solid was filtered
4. washwashed well with water
5. customdried
6. customPurification
7. washby eluting with chloroform
8. additionThe ethyl acetate eluent containing the pure product
9. concentrationwas concentrated to 2 mL volume
10. customThe crystals that separated on inducement
11. filtrationwere filtered
12. washwashed with 0.5 mL of ethyl acetate and 1 mL of ether