反应详情

温度

40 °C

(E)-4-{4-[2-(1H-indazol-3-yl)vinyl]-3-nitrophenyl}piperazine-1-carboxylic acid tert-butyl ester (0.20 g, 0.45 mmol) obtained in Step 2 was dissolved in ethanol (1.0 mL), and the solution was added with iron (0.50 g, 8.9 mmol) and water (1.0 mL) under ice-cooling, followed by stirring at 40° C. for 1 hour. To the reaction mixture under ice-cooling, water was added and the mixture was neutralized. 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)-4-{3-amino-4-[2-(1H-indazol-3-yl)vinyl]phenyl}piperazine-1-carboxylic acid tert-butyl ester (63 mg, 34%).

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