反应详情

温度

40 °C

(E)-3-{2-[4-(4-methanesulfonylpiperazin-1-yl)-2-nitrophenyl]vinyl}-1H-indazole (0.13 g, 0.29 mmol) obtained in Step 2 was dissolved in ethanol (2.0 mL), and the solution was added with tin (73 mg, 0.62 mmol) and concentrated hydrochloric acid (1.0 mL) under ice-cooling, followed by stirring at 40° C. for 1 hour. To the reaction mixture under ice-cooling, 6 mol/L aqueous sodium hydroxide solution was added to neutralize the mixture. Then, the mixture was filtered. The filtrate was added with saturated aqueous sodium hydrogencarbonate solution 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 residue was triturated in ethyl acetate to obtain (E)-2-[2-(1H-indazol-3-yl)vinyl]-5-(4-methanesulfonylpiperazin-1-yl)phenylamine (0.06 g, 52%).

1. temperaturecooling
2. temperatureTo the reaction mixture under ice-cooling
3. filtrationThen, the mixture was filtered
4. additionThe filtrate was added with saturated aqueous sodium hydrogencarbonate solution
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with water and saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was evaporated under reduced pressure
9. customThe residue was triturated in ethyl acetate