Reaktion #3283

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

benzylamine

→

pure product

Ausbeute 47.6%

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

Ausbeute 47.6%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   workup.WAITAfter 5 hours
3. 3
   Sonstigethe excess amine and dimethylformamide were evaporated at reduced pressure
4. 4
   Sonstigethe residue was triturated with a solution of 1 mL of acetone and 2 mL of petroleum ether
5. 5
   FiltrationThe tacky solid was filtered
6. 6
   Sonstigerecrystallized from ethyl acetate/petroleum ether

Vorschrift

A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido-[2,3-d]pyrimidin-7-one of Example 37, 0.50 g (4.70 mmol) of benzylamine and 0.5 mL of dimethylformamide was heated with stirring in a 120° C. oil bath. After 5 minutes, solution was complete. After 5 hours, the excess amine and dimethylformamide were evaporated at reduced pressure, and the residue was triturated with a solution of 1 mL of acetone and 2 mL of petroleum ether. The tacky solid was filtered and recrystallized from ethyl acetate/petroleum ether to give 0.092 g of pure product; mp 217°-219° C.

Quelle