反应详情

M-chloroperoxybenzoic acid (230 g) and 5-(methylthio)-2-(5-phenyl-1H-imidazol-1-yl)pyridine (118 g) were dissolved in 3 L dichloromethane, and stirred to react for 2 hours at 0° C. After the reaction was complete, 1000 mL saturated Na2S2O3 solution was added. The mixture was extracted with dichloromethane, the organic phase was washed with saturated NaCl solution, and dried with anhydrous sodium sulfate. After filtration and concentration, the crude product was purified by column chromatography to obtain the target compound (50 g). 1H-NMR (300 MHz, CDCl3): δ 3.14 (3H, s), 6.90 (1H, d), 7.24 (3H, m), 7.39 (3H, m), 8.06 (1H, dd), 8.30 (1H, s), 9.05 (1H, d); LC-MS m/z: 300 [M++1], purity (HPLC)>95%.

1. customto react for 2 hours at 0° C
2. extractionThe mixture was extracted with dichloromethane
3. washthe organic phase was washed with saturated NaCl solution
4. dry with materialdried with anhydrous sodium sulfate
5. filtrationAfter filtration and concentration
6. customthe crude product was purified by column chromatography