反应详情

温度

180 °C

A mixture of 0.155 g (0.40 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.500 g (4.10 mmol) of 3-(hydroxymethyl)aniline was heated in a 180° C. oil bath for 10 minutes. At ca. 120° C., 2 mL of glacial acetic acid were added to dissolve the gum. Water (20 mL) was added to precipitate a solid. The mixture was filtered. The cake was washed well with water and dried; wt 0.130 g. Purification was effected by silica gel chromatography eluting with chloroform and then with ethyl acetate to obtain the fraction containing the pure product. The ethyl acetate eluent was concentrated to 1 mL volume. The crystals that separated one inducement were filtered and washed with 0.5 mL of ethyl acetate and then 1 mL of ether; wt 0.059 g; mp 215°-217° C.

1. dissolutionto dissolve the gum
2. customto precipitate a solid
3. filtrationThe mixture was filtered
4. washThe cake was washed well with water
5. customdried
6. customPurification
7. washeluting with chloroform
8. customwith ethyl acetate to obtain the fraction
9. additioncontaining the pure product
10. concentrationThe ethyl acetate eluent was concentrated to 1 mL volume
11. customThe crystals that separated one inducement
12. filtrationwere filtered
13. washwashed with 0.5 mL of ethyl acetate