反应详情

To a solution of the 1H-indazole-5-carboxylic acid (281 mg, 1.73 mmol) obtained in Reference Example 1 in N,N-dimethylformamide (10 ml) were added 1-benzyl-N-methylpiperidin-4-amine (390 mg, 1.91 mmol), triethylamine (0.29 ml, 2.08 mmol), 1-ethyl-3-(3′-dimethylaminopropyl)-carbodiimide monohydrochloride (499 mg, 2.60 mmol) and hydroxybenzotriazole (281 mg, 2.08 mmol), and the resulting mixture was stirred overnight at room temperature. An aqueous sodium hydrogencarbonate solution was added to the reaction solution, followed by extraction with chloroform, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: chloroform/ethyl acetate→chloroform/methanol) to obtain N-(1-benzylpiperidin-4-yl)-N-methyl-1H-indazole-5-carboxamide (502 mg, 83%).

1. extractionfollowed by extraction with chloroform
2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
3. concentrationThe solvent was concentrated under reduced pressure
4. customthe resulting residue was purified by a silica gel column chromatography (eluent: chloroform/ethyl acetate→chloroform/methanol)