反应详情

温度

50 °C

Sodium thiomethoxide (1.06 g, 15.2 mmol) was added at 25° C. to 4-Nitro-[2,2′]bipyridinyl 1-oxide (3.0 g, 13.8 mmol) in dimethyl formamide (15 mL) and stirred for 2 hours at 50° C. The reaction mixture was added into ice (200 g) under vigorous stirring, the solid formed was filtered and washed with water (100 mL) and ether (100 mL), the filtrate was concentrated, diluted with water, extracted with dichloromethane (3×100 mL), dried with anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude was purified by column chromatography on silica gel (0-100% Ethyl acetate in Hexane) to afford 4-methylsulfanyl-[2,2′]bipyridinyl 1-oxide as a white solid (650.0 mg, 22%).

1. customthe solid formed
2. filtrationwas filtered
3. washwashed with water (100 mL) and ether (100 mL)
4. concentrationthe filtrate was concentrated
5. additiondiluted with water
6. extractionextracted with dichloromethane (3×100 mL)
7. dry with materialdried with anhydrous sodium sulphate
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe crude was purified by column chromatography on silica gel (0-100% Ethyl acetate in Hexane)