反应详情

温度

80 °C

PdCl2(dppf)CH2Cl2 (39 mg) was added to a mixture of tert-butyl 3-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)azetidine-1-carboxylate (200 mg) obtained in Step 2 above, 1-ethynyl-3,5-dimethoxybenzene (117 mg), copper (I) iodide (14 mg), and triethylamine (0.5 ml) in THF (5 ml). After nitrogen purging, the resulting mixture was stirred at 80° C. for 1.5 hours. Ethyl acetate and water were added to the reaction mixture to separate the organic layer. After being washed with a saturated sodium chloride solution, the organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The resulting residue was purified by basic silica gel column chromatography (developing solvent: hexane/ethyl acetate) to obtain the title compound as a colorless, amorphous substance (185 mg). Physical properties: m/z [M+H]+ 451.1

1. customto separate the organic layer
2. washAfter being washed with a saturated sodium chloride solution
3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe resulting residue was purified by basic silica gel column chromatography (developing solvent: hexane/ethyl acetate)