反应详情

温度

0 °C

4-(4-Amino-3-bromo-5-nitro-phenyl)-2-methyl-5-oxo-7-propyl-1,4,5,6,7,8-hexahydro-quinoline-3-carbonitrile (600 mg) was dissolved in THF (150 ml) and cooled to 0° C. Acetic acid (1.3 ml) was added, followed by addition of zinc dust (2 g). The resulting slurry was stirred at 0° C. for 2 h, and then another 4 h at room temperature. The mixture was filtered and diluted with saturated aq. NaHCO3, followed by extraction with ethyl acetate. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by chromatography on silicagel in heptane/ethyl acetate 3/1→0/1 (v/v) as eluent.

1. customanother 4 h
2. customat room temperature
3. filtrationThe mixture was filtered
4. additiondiluted with saturated aq. NaHCO3
5. extractionfollowed by extraction with ethyl acetate
6. dry with materialThe organic layer was dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was purified by chromatography on silicagel in heptane/ethyl acetate 3/1→0/1 (v/v) as eluent