反应详情

To a solution of dimethyl[2-(4-fluoro-2-nitrophenyl)-1-phenylethyl]malonate (8a) (5.0 g) in methanol (20 mL) was added ammonium chloride (1.5 g) and zinc dust (11.0 g). The reaction mixture was then heated to reflux for 1 h. The reaction mixture was filtered through a diatomaceous earth pad, and the organic solvents were removed in vacuo. The resulting yellow oil was dissolved in ethyl acetate (100 mL) and washed with saturated aqueous potassium carbonate solution (2×), the organic layer was dried, filtered, and concentrated in vacuo to afford the title compound as a tan gum (4.1 g, 90%). MS APCI, m/z=346 (M+1). LC/MS: 2.51 min.

1. temperatureThe reaction mixture was then heated
2. temperatureto reflux for 1 h
3. filtrationThe reaction mixture was filtered through a diatomaceous earth pad
4. customthe organic solvents were removed in vacuo
5. dissolutionThe resulting yellow oil was dissolved in ethyl acetate (100 mL)
6. washwashed with saturated aqueous potassium carbonate solution (2×)
7. customthe organic layer was dried
8. filtrationfiltered
9. concentrationconcentrated in vacuo