反应详情

温度

120 °C

To a solution of 1-(2-methylcyclopentyl)-3-methyl-5-amino-1H-pyrazole-4-carboxamide (2.3 g, 10.4 mmol) in xylenes (8.0 ml) under argon was added 4-pyridinecarboxaldehyde (1.5 ml, 15.5 mmol). The reaction mixture was warmed to 120° C. and stirred for 1 hour at which time the mixture became homogeneous. The reaction mixture was then heated to 160° C. for 24 hours and then cooled to room temperature. A solid precipitated which was collected by filtration through a glass frit. The solid was washed with ether, saturated NaHCO3 then water and was recrystallized from DMF. The solid was collected on a glass frit and was washed with methanol, then ether and dried at 110° C. for 72 hours in high vacuum to afford 1.05 g (33%) of 1-(2-methylcyclopentyl)-3-methyl-6-(4-pyridyl)-pyrazolo[3,4-d]pyrimidin-4-one as white crystals m.p. 290°-291° C.

1. temperatureThe reaction mixture was then heated to 160° C. for 24 hours
2. temperaturecooled to room temperature
3. customA solid precipitated which
4. filtrationwas collected by filtration through a glass frit
5. washThe solid was washed with ether, saturated NaHCO3
6. customwater and was recrystallized from DMF
7. customThe solid was collected on a glass frit
8. washwas washed with methanol
9. dry with materialether and dried at 110° C. for 72 hours in high vacuum