反应详情

The compound of example 391 (1.5 g, 0.0040 mol), iron (0.533 g, 0.0095 mol) and ammonium chloride (0.930 g, 0.0174 mol) in EtOH: H2O (22.5 mL, 15:7.5) was refluxed for about 16 h. After completion of the reaction, the reaction mixture was filtered through celite. The filtrate was concentrated to obtain a residue which was dissolved in ethyl acetate and washed with water and brine, dried over anhydrous sodium sulfate and concentrated to obtain a residue, which was purified by column chromatography (silica gel, 30% ethyl acetate in petroleum ether) to obtain the title compound.

1. customAfter completion of the reaction
2. filtrationthe reaction mixture was filtered through celite
3. concentrationThe filtrate was concentrated
4. customto obtain a residue which
5. washwashed with water and brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated
8. customto obtain a residue, which
9. customwas purified by column chromatography (silica gel, 30% ethyl acetate in petroleum ether)