反应详情

温度

160 °C

A mixture of 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (1.05 g, 4.73 mmol), 3-[2-(4-morpholinyl)ethoxy]benzaldehyde (1.67 g) and xylenes (7 ml) was heated to 160° C. overnight. Additional aldehyde (0.4 g) was added and the mixture was heated at 160° C. until the reaction was complete. The reaction mixture was cooled to room temperature and a solid formed which was collected by filtration and washed with ether. The filtrate was concentrated to dryness and the residue was combined with the solid and was purified by column chromatography on silica gel eluting with ethyl acetate/ethanol (60/40). The solid product thus obtained was washed with ether, recrystallized from ethyl acetate and then washed with ether again to afford 1-cyclopentyl-3-ethyl-6-[3-[2-(4-morpholinyl)ethoxy]phenyl]-pyrazolo[3,4-d]pyrimidin-4-one, m.p. 173-176° C.

1. temperaturethe mixture was heated at 160° C. until the reaction
2. temperatureThe reaction mixture was cooled to room temperature
3. customa solid formed which
4. filtrationwas collected by filtration
5. washwashed with ether
6. concentrationThe filtrate was concentrated to dryness
7. customwas purified by column chromatography on silica gel eluting with ethyl acetate/ethanol (60/40)
8. customThe solid product thus obtained
9. washwas washed with ether
10. customrecrystallized from ethyl acetate
11. washwashed with ether again