反应详情

To a solution of 4-(4-methanesulfonylpiperazin-1-yl)-2-nitrobenzaldehyde (0.36 g, 1.1 mmol) obtained in Step 1 in methanol (5.0 mL), (1H-indazol-3-ylmethyl) triphenylphosphonium bromide (0.54 g, 1.1 mmol) and potassium carbonate (0.31 g, 2.3 mmol) were added, followed by stirring at room temperature for 1 hour. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The filtrate was purified by silica gel column chromatography (hexane/ethyl acetate=4/1 to ethyl acetate) to obtain (E)-3-{2-[4-(4-methanesulfonylpiperazin-1-yl)-2-nitrophenyl]vinyl}-1H-indazole (0.48 g, 26%).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe filtrate was purified by silica gel column chromatography (hexane/ethyl acetate=4/1 to ethyl acetate)