反应详情

温度

120 °C

A microwave vial was charged with Solvias catalyst (7 mg), tripotassium phosphate (84 mg) and 4-bromo-1H-pyrrolo[2,3-c]pyridine (from prep such as in US2005/0090529, 29 mg). 1-(1-methylethyl)-N-[2-(tetrahydro-2H-pyran-2-yl)-6-(4,4,6,6-tetramethyl-1,3,2-dioxaborinan-2-yl)-2H-indazol-4-yl]-1H-pyrazole-5-carboxamide (65 mg) in 1,4-dioxane (0.5 ml) was added, followed by water (0.1 ml) and the reaction was heated under microwave irradiation for a total of 30 min at 120° C. The reaction was washed through a silica cartridge preconditioned with methanol, with methanol. The solvent was removed under a stream of nitrogen, then washed with DCM and water. The resultant solution was evaporated under a stream of nitrogen. The residue was dissolved in DMSO:methanol (1 ml, 1:1, v/v) and purified by MDAP (method A). Appropriate fractions were dried under a stream of nitrogen. The residue was dissolved in methanol, 2M HCl (aq) (3 drops) was added and the solution was left to stand for 60 min. The solvent was removed under a stream of nitrogen and the residue was dissolved in methanol, washed with methanol through an aminopropyl cartridge preconditioned with methanol and dried under a stream of nitrogen to give title compound, 5 mg.

1. washThe reaction was washed through a silica cartridge
2. customThe solvent was removed under a stream of nitrogen
3. washwashed with DCM and water
4. customThe resultant solution was evaporated under a stream of nitrogen
5. dissolutionThe residue was dissolved in DMSO
6. custommethanol (1 ml, 1:1, v/v) and purified by MDAP (method A)
7. customAppropriate fractions were dried under a stream of nitrogen
8. dissolutionThe residue was dissolved in methanol
9. addition2M HCl (aq) (3 drops) was added
10. waitthe solution was left
11. customThe solvent was removed under a stream of nitrogen
12. dissolutionthe residue was dissolved in methanol
13. washwashed with methanol through an aminopropyl cartridge
14. customdried under a stream of nitrogen