反应详情

温度

100 °C

A mixture of 6-benzyl-pyridine-3-carbaldehyde (4.7 g, 24 mmol) described in Manufacturing Example 210-1-4, nitromethane (7.3 g, 120 mmol), ammonium acetate (5.6 g, 72 mmol), and acetic acid (40 mL) was stirred for 90 minutes at 100° C. The reaction solution was partitioned into ethyl acetate and water. The organic layer was washed with saturated aqueous sodium bicarbonate and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1) to obtain the title compound (1.2 g, 21%).

1. customThe reaction solution was partitioned into ethyl acetate and water
2. washThe organic layer was washed with saturated aqueous sodium bicarbonate
3. concentrationconcentrated under a reduced pressure
4. customThe residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1)