Reaktion #3282

Reaktionsgleichung

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

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

n-butylamine

→

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

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   TemperaturAfter 20 hours reflux
3. 3
   Sonstigethe excess amine and dimethylformamide were evaporated
4. 4
   Sonstigethe residue was triturated with water
5. 5
   Filtrationfiltered
6. 6
   Waschenwashed with water
7. 7
   Sonstigedried
8. 8
   SonstigeRecrystallization from ethyl acetate/petroleum ether
9. 9
   Sonstigegave pure product

Vorschrift

A mixture of 0.177 g (0.50 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 10 mL of n-butylamine and 1.0 mL of dimethylformamide was heated with stirring to reflux (110° C. oil bath). After 1 hour, solution was complete. After 20 hours reflux, the excess amine and dimethylformamide were evaporated, and the residue was triturated with water, filtered, washed with water, and dried; wt 0.180 g. Recrystallization from ethyl acetate/petroleum ether gave pure product; wt 0.116 g; mp 184°-186° C.

Quelle