反应详情

温度

80 °C

To a two necked 250 mL round bottom flask, charged with 1-[5-(2,4-Dichlorophenylsulfanyl)-4-nitro-2-thienyl]ethanone (7.0 g, 20.2 mmol) prepared as in example 2, 50 mL ethanol and 50 mL of water followed by ammonium chloride (4.32 g, 80.8 mmol) and iron powder (4.53 g, 80.8 mmol). The resulting reaction mixture was heated at 80° C. for 2 hours. After this time, the reaction mixture was cooled to ambient temperature and was passed through a cellite cartridge. The filtrate was concentrated and water was added to the residue and extracted with ethyl acetate. The combined organic layer was separated, dried (Na2SO4), filtered and concentrated to afford the title product (6.4 g, 78% yield). 1H NMR (400 MHz, d6-DMSO) δ: 7.64 (1H, s), 7.44 (1H, s), 7.37 (1H, m), 6.68 (1H, m), 2.50 (3H, s).

1. customThe resulting reaction mixture
2. temperatureAfter this time, the reaction mixture was cooled to ambient temperature
3. concentrationThe filtrate was concentrated
4. additionwater was added to the residue
5. extractionextracted with ethyl acetate
6. customThe combined organic layer was separated
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated