反应详情

A suspension of tert-butyl 3-(methylsulfonyloxy)azetidine-1-carboxylate (1.32 g) obtained in Step 1 above, 3-iodo-1H-pyrazolo[3,4-d]pyrimidin-4-amine (1.37 g), and cesium carbonate (3.47 g) in DMF (10 ml) was stirred at 90° C. for 10 hours. Ethyl acetate and water were added thereto to separate the organic layer. 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 light-yellow amorphous substance (482 mg). Physical properties: m/z [M+H]+ 417.0

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