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-b]pyridine (commercial from Sinova, 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 10 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, 2 M HCl (aq) (3 drops) was added and the solution was left to stand for 30 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, 20 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. addition2 M 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