反应详情

温度

55 °C

To a mixture of biphenyl-3-yl-acetohydroximoyl chloride (120 mg) described in Manufacturing Example 85-1-3 and tetrahydrofuran (6 mL) were added 3-ethynyl-pyridin-2-ylamine (28 mg, 0.24 mmol) described in Manufacturing Example 1-2-3 and triethylamine (200 μL, 1.4 mmol) at room temperature, which was stirred for 2.5 hours at 55° C. The reaction mixture was cooled to room temperature and water was added at that temperature, followed by extraction with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and was concentrated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=2:1) to obtain the title compound (27 mg, 34%).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with saturated aqueous sodium chloride
4. concentrationwas concentrated under a reduced pressure
5. customThe residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=2:1)