反应详情

To a suspension of 1-benzenesulfonyl-3-(l -phenoxycarbonyl-4-piperazinyl)-1 H-indazole (31.3 g, 67.7 mmol) in ethanol (500 ml) was added ,50% KOH (aq.) (100 g of KOH in 100 g H2O) at room temperature. The reaction mixture was warmed to reflux for 6.5 hours and cooled to room temperature. After adjusting the pH to about two using HCl (con., 120 ml), the volatiles were removed under reduced pressure. The remaining residue was diluted with water and removed via filtration. The aqueous filtrate was washed with EtOAc and basified to pH=8 using 50% NaOH (aq.). The product was extracted into 10:1 dichloromethane/isopropylalcohol. The combined organics were dried (MgSO4), filtered, and concentrated to give 13.0 g of desired 3-piperazin-1-yl-1 H-indazole as a brown solid which was used without further purification.

1. additionwas added
2. customat room temperature
3. temperatureThe reaction mixture was warmed
4. temperatureto reflux for 6.5 hours
5. customthe volatiles were removed under reduced pressure
6. additionThe remaining residue was diluted with water
7. customremoved via filtration
8. washThe aqueous filtrate was washed with EtOAc and basified to pH=8
9. extractionThe product was extracted into 10:1 dichloromethane/isopropylalcohol
10. dry with materialThe combined organics were dried (MgSO4)
11. filtrationfiltered
12. concentrationconcentrated