反応 #3289

反応方程式

6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

6-(2,6-Dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

aniline

→

6-(2,6-Dichlorophenyl)-8-methyl-2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

反応条件

後処理

1. 1
   その他Most of the excess aniline was evaporated at reduced pressure
2. 2
   workup.DISSOLUTIONThe remaining gum was dissolved in 1.0 mL of ethyl acetate
3. 3
   その他Further purification
4. 4
   その他to remove dark colors
5. 5
   洗浄eluting with chloroform
6. 6
   その他50% hexane-ethyl acetate to obtain pure crystalline product

実験手順

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.

出典