反应详情

温度

75 °C

To a solution of the 5-bromo-1-tetrahydro-2H-pyran-2-yl-1H-indazole (250 mg, 0.889 mmol) obtained in Reference Example 5 in toluene (12 ml) were added 1-benzylpiperazine (0.24 ml, 1.35 mmol) and sodium tert-butoxide (128 mg, 1.33 mmol) at room temperature. After deaeration, bis(tri-o-tolylphosphine)-palladium(II) dichloride (70 mg, 0.0891 mmol) was added thereto and the resulting mixture was stirred at 75° C. for three and a half hours. Then, the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: chloroform/ethyl acetate=5/2) to obtain 5-(4-benzyl-1-piperazinyl)-1-tetrahydro-2H-pyran-2-yl-1H-indazole (183 mg, 55%).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with a saturated aqueous sodium chloride solution
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customthe resulting residue was purified by a silica gel column chromatography (eluent: chloroform/ethyl acetate=5/2)