反应详情

温度

50 °C

To a tetrahydrofuran (5 mL) solution of 3-ethynyl-pyridin-2,6-diamine (20 mg, 0.15 mmol) described in Manufacturing Example 13-1-3 and 2-(6-benzyl-pyridin-3-yl)-acetohydroximoyl chloride (79 mg, 0.30 mmol) described in Manufacturing Example 210-1-7 was added triethylamine (46 mg, 0.45 mmol), which was stirred for 30 minutes at 50° C. The reaction solution was cooled to room temperature and partitioned into ethyl acetate and water. The organic layer was separated and concentrated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate, then ethyl acetate: methanol=20:1) to obtain the title compound (43 mg, 80%).

1. temperatureThe reaction solution was cooled to room temperature
2. custompartitioned into ethyl acetate and water
3. customThe organic layer was separated
4. concentrationconcentrated under a reduced pressure
5. customThe residue was purified by NH silica gel column chromatography (ethyl acetate