反应详情

温度

60 °C

To a tetrahydrofuran (5.00 mL) solution of (5-(4-methyl-benzyl)-thiophen-2-yl)acetohydroximoyl chloride (250 mg, 0.894 mmol) described in Manufacturing Example 92-1-5 and 3-ethynyl-pyridin-2,6-diamine (50.0 mg, 0.376 mmol) described in Manufacturing Example 13-1-3 was added triethylamine (157 μL, 1.13 mmol) at room temperature, which was stirred for 30 minutes at 60° C. Water was added to the reaction solution at room temperature, which was extracted with ethyl acetate. The organic layer was washed with 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→3:1) to obtain the title compound (49.8 mg, 35.2%).

1. extractionwhich was extracted with ethyl acetate
2. washThe organic layer was washed with saturated aqueous sodium chloride
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated under a reduced pressure
5. customThe residue was purified by NH silica gel column chromatography (ethyl acetate: heptane=2:1→3:1)