Reaktion #3294

Reaktionsgleichung

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

4-methylaniline

→

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   TemperaturThe resulting solution was heated for 10 minutes
3. 3
   SonstigeMuch of the excess 4-methylaniline was evaporated at reduced pressure
4. 4
   workup.DISSOLUTIONThe remainder was dissolved in 1 mL of ethyl acetate
5. 5
   SonstigeThe crystals that separated from the dark solution
6. 6
   Filtrationwere filtered
7. 7
   Waschenwashed with 2 mL of ethyl acetate
8. 8
   SonstigeRecrystallization from ethyl acetate
9. 9
   Sonstigegave pure product

Vorschrift

A mixture 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 and 0.50 g (4.70 mmol) of 4-methylaniline was heated, with stirring, in a 180° C. oil bath. The resulting solution was heated for 10 minutes. Much of the excess 4-methylaniline was evaporated at reduced pressure. The remainder was dissolved in 1 mL of ethyl acetate. The crystals that separated from the dark solution were filtered and washed with 2 mL of ethyl acetate and then ether; wt 0.111 g. Recrystallization from ethyl acetate gave pure product; wt 0.050 g; mp 243°-245° C.

Quelle