反应详情

温度

80 °C

After suspending 6,7-dimethoxy-4-(5-nitrothiophen-2-ylsulfanyl)quinoline (1.39 g, 4.00 mmol), iron (1.12 g, 20.0 mmol) and ammonium chloride (2.18 g, 40.0 mmol) in an ethanol (32 ml)-water (8 ml) mixed solvent, the suspension was heated and stirred at 80° C. for 5 minutes. After completion of the reaction, the reaction mixture was filtered with celite and washed in ethyl acetate. The organic layer was washed with water and saturated saline and dried over anhydrous magnesium sulfate, the drying agent was filtered off and the filtrate was distilled off under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (eluent-ethyl acetate:hexane=3:1), and the fraction containing the target substance was concentrated to obtain the title compound (1.93 g, 5.54 mmol, 55%) as yellowish-brown crystals.

1. additionmixed solvent
2. temperaturethe suspension was heated
3. customAfter completion of the reaction
4. filtrationthe reaction mixture was filtered with celite
5. washwashed in ethyl acetate
6. washThe organic layer was washed with water and saturated saline
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationthe drying agent was filtered off
9. distillationthe filtrate was distilled off under reduced pressure
10. customThe obtained crude product
11. additionthe fraction containing the target substance
12. concentrationwas concentrated