反应详情

温度

120 °C

A microwave vial was charged with Solvias catalyst (8 mg), tripotassium phosphate (90 mg) and 7-bromo-1,3-benzoxazol-2(3H)-one (from prep. such as US2006/0122189A1, 33 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 (70 mg) in 1,4-dioxane (0.5 ml) was added followed by water (0.1 ml). The reaction was heated under microwave irradiation at 120° C. for 10 min. The reaction was passed through a silica cartridge preconditioned with methanol, washing with methanol, then dried under a stream of nitrogen. The residue was subjected to a DCM/water wash and then dried 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 evaporated under a stream of nitrogen. The residues were dissolved in a minimum amount of methanol and combined. A few drops of 2M HCl (aq) were added and the reaction was left to stand at room temperature. The reaction was then evaporated under a stream of nitrogen, passed through an aminopropyl cartridge and dried to give title compound, 10 mg.

1. washwashing with methanol
2. customdried under a stream of nitrogen
3. washwash
4. customdried 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 evaporated under a stream of nitrogen
8. dissolutionThe residues were dissolved in a minimum amount of methanol
9. additionA few drops of 2M HCl (aq) were added
10. waitthe reaction was left
11. customto stand at room temperature
12. customThe reaction was then evaporated under a stream of nitrogen
13. customdried