反应详情

温度

95 °C

7-Chloro-N-(3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-yl)imidazo[1,2-a]pyridine-3-carboxamide (5.0 g, 10.9 mmol), potassium hydroxide (3.38 g, 60.2 mmol), DMSO (50 mL), and 2-(4-methylpiperazin-1-yl)ethanol (3.16 g, 21.9 mmol) were combined under nitrogen and heated to 95° C. for 16 hours. The mixture was cooled to ambient temperature and THF (300 mL) was added. The slurry was stirred at ambient temperature for 3 hours. The solids were filtered off and the THF removed from the filtrates under vacuum to give a DMSO solution of the product. The DMSO solution was heated to 60° C. and water (100 mL) was added to precipitate out the product. The slurry was cooled to ambient temperature and stirred for 18 hours. The solids were collected by filtration and washed with water (100 mL) and MTBE (50 mL). The material was dried under vacuum at 40° C. to give N-(3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-yl)-7-(2-(4-methylpiperazin-1-yl)ethoxy)imidazo[1,2-a]pyridine-3-carboxamide (4.54 g). MS (ES+APCI) m/z=565.1 (M+H).

1. temperatureThe mixture was cooled to ambient temperature
2. filtrationThe solids were filtered off
3. customthe THF removed from the filtrates under vacuum
4. customto give a DMSO solution of the product
5. customto precipitate out the product
6. temperatureThe slurry was cooled to ambient temperature
7. stirringstirred for 18 hours
8. filtrationThe solids were collected by filtration
9. washwashed with water (100 mL) and MTBE (50 mL)
10. customThe material was dried under vacuum at 40° C.