反应详情

温度

98 °C

8-Cyclopentyl-6-fluoro-2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one (2.0 g, 6.77 mmol, prepared accoring to Example 16) and 5 4-(6-Amino-pyridin-3-yl)-piperazine-1-carboxylic acid tert-butyl ester (6.0 g, 21 mmol) were added to toluene (8 ml) and heated to 98° C. for 18 hours. The mixture was filtered, washed with toluene and the solid suspended in diethyl ether. The mixture was filtered and the solid was dissolved in chloroform, washed with 1 N citric acid, brine and dried over anhydrous magnesium sulfate. The crude product was triturated with diethyl ether and dried in vacuo to provide 4-[6-(8-cyclopentyl-6-fluoro-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester as a solid (0.88 g, 25%). MS (APCI) M++1: Calc'd, 510.3. Found 510.2.

1. filtrationThe mixture was filtered
2. washwashed with toluene
3. filtrationThe mixture was filtered
4. dissolutionthe solid was dissolved in chloroform
5. washwashed with 1 N citric acid, brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe crude product was triturated with diethyl ether
8. customdried in vacuo