反应详情

To a solution of 3-(1H-pyrazol-4-yl)-pyridin-2,6-diamine (25 mg, 0.14 mmol) described in Manufacturing Example 36-1-2 in N,N-dimethylformamide (3 mL) was added sodium hydride (8.6 mg, 0.22 mmol, 60% in oil) under nitrogen atmosphere on an ice bath (0° C.). Following 30 minutes of stirring at room temperature, 2-(4-chloromethyl-benzyloxy)-pyridine (43.4 mg, 0.19 mmol) described in Manufacturing Example 30-1-1 was added and stirred for 30 minutes at 60° C. The reaction mixture was partitioned into water and ethyl acetate at room temperature. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=2:1, then ethyl acetate only) to obtain the title compound (22.8 mg, 43%).

1. additionwas added
2. stirringstirred for 30 minutes at 60° C
3. customThe reaction mixture was partitioned into water and ethyl acetate at room temperature
4. washThe organic layer was washed with water and saturated aqueous sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was evaporated under a reduced pressure
7. customThe residue was purified by NH silica gel column chromatography (ethyl acetate