反应详情

To a solution of 2-(4-((E)-2-nitro-vinyl)-phenoxy)-pyridine (9.9 g, 41 mmol) described in Manufacturing Example 209-1-2, acetic acid (2.5 g) and dimethyl sulfoxide (60 mL) was added sodium borohydride (770 mg, 20 mmol) while the temperature was held at 30° C. or lower, which was stirred for 15 minutes at room temperature. This reaction solution was partitioned into ethyl acetate and water while the temperature was held at 30° C. or lower. The organic layer was separated and concentrated under reduced pressure. The residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=3:1) to obtain the title compound (4.5 g, 45%).

1. customwas held at 30° C.
2. customThis reaction solution was partitioned into ethyl acetate and water while the temperature
3. customwas held at 30° C.
4. customThe organic layer was separated
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=3:1)