反应详情

The compound of example 5 (0.9 g, 0.00244 mol), iron (0.32 g, 0.0057 mol) and ammonium chloride (0.551 g, 0.0103 mol) were taken in EtOH:THF:H2O (15.5 mL, 9:4.5:2.25). The reaction mixture 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 solid residue which was dissolved in ethyl acetate and washed with water and brine, dried over anhydrous sodium sulfate and concentrated to obtain a crude product, which was purified by column chromatography (silicagel, 30% ethyl acetate in petroleum ether).

1. temperatureThe reaction mixture was refluxed for about 16 h
2. customAfter completion of the reaction
3. filtrationthe reaction mixture was filtered through celite
4. concentrationThe filtrate was concentrated
5. customto obtain a solid residue which
6. washwashed with water and brine
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated