反应详情

温度

184 °C

A solution of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 in 1.00 g (10.70 mmol) of aniline was maintained at reflux (184° C.) for 3 minutes. Most of the excess aniline was evaporated at reduced pressure. The remaining gum was dissolved in 1.0 mL of ethyl acetate. Crystals developed on inducement; wt 0.088 g. Further purification to remove dark colors was effected by silica gel chromatography, eluting with chloroform and then 50% hexane-ethyl acetate to obtain pure crystalline product; wt 0.046 g; mp 247°-249° C.

1. customMost of the excess aniline was evaporated at reduced pressure
2. dissolutionThe remaining gum was dissolved in 1.0 mL of ethyl acetate
3. customFurther purification
4. customto remove dark colors
5. washeluting with chloroform
6. custom50% hexane-ethyl acetate to obtain pure crystalline product