反应详情

A mixture of 6-(4-benzyloxy-2-fluoro-phenyl)-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acid (304 mg), amine (200 (200 mg), DIPEA (340 μL) and BEP (190 mg) in dichloroethane (6.5 mL) was stirred at r.t. for 90 min. The solvent was distilled off in vacuo, the residue was re-dissolved in ethyl acetate (20 mL) and washed twice with water, twice with saturated sodium bicarbonate solution and with brine, then dried over magnesium sulfate. After evaporation of the solvents, the residue was purified by flash chromatography (silica, heptane/ethyl acetate gradient) giving 278 mg (59%) of the title compound.

1. distillationThe solvent was distilled off in vacuo
2. dissolutionthe residue was re-dissolved in ethyl acetate (20 mL)
3. washwashed twice with water, twice with saturated sodium bicarbonate solution and with brine
4. dry with materialdried over magnesium sulfate
5. customAfter evaporation of the solvents
6. customthe residue was purified by flash chromatography (silica, heptane/ethyl acetate gradient)